A method for preparing an antioxidant hydrogel-based facial mask

Abstract

The application relates to the technical field of masks and discloses a preparation method of an antioxidant hydrogel-based mask, which comprises the following steps: adding grape seed white and extract liquid, coconut water, tannic acid and the like into hyaluronic acid hydrogel to swell, drying, grinding and sieving to obtain modified hydrogel powder. Polylactic acid is used as raw material, a solution spray spinning method is adopted, and then surface plasma treatment is carried out to obtain amino-modified polylactic acid nanofiber film. The nanofiber film is treated by using glutaraldehyde to introduce aldehyde groups on the surface of the fiber film, and spermidine is grafted to obtain spermidine-modified polylactic acid nanofiber. Finally, the modified hydrogel powder is added into deionized water and stirred and dispersed, the spermidine-modified polylactic acid nanofiber film is immersed in the deionized water, fully stirred and uniformly mixed, and then taken out to obtain the antioxidant hydrogel-based mask. The hydrogel-based mask prepared by the application has good antioxidant performance and moisturizing performance.

Description

Technical Field

[0001] This invention relates to the field of facial mask technology, specifically to a method for preparing an antioxidant hydrogel-based facial mask. Background Technology

[0002] With the rapid development of the national economy, people are paying more and more attention to self-care, and facial masks have become an indispensable part of this. Nanofiber membranes, due to their high porosity, large surface area, and controllable morphology, are widely used in daily necessities. However, nanofiber membranes suffer from poor moisturizing properties and poor adhesion, thus requiring improvements in their moisturizing properties and adhesion to expand their applications. Hydrogels are three-dimensional cross-linked polymer materials with high water content, good moisturizing properties, biocompatibility, and functionality; however, traditional hydrogels have poor biocompatibility.

[0003] Polylactic acid (PLA) is a biodegradable polymer material widely used in biomedicine and materials fields. However, its high crystallinity, lack of active reactive groups, poor hydrophilicity, and weak cell adhesion greatly limit its application range. Furthermore, PLA nanofiber membranes prepared from PLA also have poor hydrophilicity. Summary of the Invention

[0004] (a) Technical problems to be solved

[0005] To address the shortcomings of existing technologies, this invention provides a method for preparing an antioxidant hydrogel-based face mask. By combining a modified polylactic acid nanofiber membrane with a modified hydrogel, the advantages of both can be integrated to prepare a moisturizing and antioxidant face mask.

[0006] (II) Technical Solution

[0007] A method for preparing an antioxidant hydrogel-based face mask, wherein the method for preparing the antioxidant hydrogel-based face mask is as follows:

[0008] Add the modified hydrogel powder to deionized water, stir and disperse to prepare a 5-15% solution, then immerse the spermidine-modified polylactic acid nanofiber membrane in it, stir and mix thoroughly, and take it out to obtain an antioxidant hydrogel-based face mask.

[0009] Preferably, the preparation method of the spermidine-modified polylactic acid nanofiber membrane is as follows:

[0010] S1. Polylactic acid is added to a 5% (w / w) ethanol-dichloromethane solution, stirred and dissolved, and polylactic acid nanofiber membrane is prepared by solution spray spinning. After drying, it is placed in the cavity of a plasma surface active agent for surface plasma treatment to obtain an amino-modified polylactic acid nanofiber membrane.

[0011] S2. Immerse the amino-modified polylactic acid nanofiber membrane in an aqueous solution of glutaraldehyde at 30-35℃ for 2-4 hours, wash with deionized water, dry, then add 2-5% (w / w) of spermidine aqueous solution and soak for 5-12 hours. After the reaction is complete, wash with deionized water and dry to obtain the spermidine-modified polylactic acid nanofiber membrane.

[0012] More preferably, in S1, the airflow pressure in the solution spray spinning method is 0.2 MPa, the receiving distance is 20 cm, and the nozzle diameter is 0.5 mm.

[0013] More preferably, in step S1, the control conditions of the plasma surface active agent are: under ammonia conditions, processing at a power of 50W for 30 seconds.

[0014] More preferably, in S2, the mass fraction of the glutaraldehyde aqueous solution is 5-10%.

[0015] Preferably, the method for preparing the modified hydrogel powder is as follows:

[0016] (1) Place grape seed powder and Bletilla striata powder in a container, add 40-60% ethanol aqueous solution, stir and disperse, place in a flash extraction device, and extract using flash extraction technology. After extraction, separate and filter to obtain grape seed and Bletilla striata extract. The flash extraction process is as follows: extraction voltage is 100-150V, extraction times are 2-4 times, and extraction time is 30-60s.

[0017] (2) Add grape seed extract, coconut water, tannic acid, and allantoin skin care agent to hyaluronic acid hydrogel, swell and shake at room temperature for 24 hours, take it out, wash with deionized water, dry, grind and sieve to obtain modified hydrogel powder.

[0018] The grape seeds, Bletilla striata, and coconut water mentioned are all commercially available.

[0019] The grape seeds are rich in polyphenols, flavonoids and other active substances. As a natural and highly effective antioxidant, they can eliminate reactive oxygen species generated by oxidative stress. They are extracted using a flash extraction process and added to a face mask to enhance the mask's antioxidant and anti-aging effects.

[0020] Bletilla striata is a traditional Chinese medicine containing Bletilla striata polysaccharide. Bletilla striata polysaccharide has a good scavenging effect on hydroxyl radicals and superoxide anion radicals. It is extracted using a flash extraction process and added to the face mask to enhance the antioxidant and anti-aging effects of the face mask.

[0021] The coconut water is extracted from fresh coconuts and has good antioxidant capacity. It has a strong ability to scavenge superoxide anion free radicals, hydroxyl free radicals, and DPPH free radicals. Therefore, adding it to a face mask can enhance the antioxidant and anti-aging effects of the mask.

[0022] The tannic acid is a natural water-soluble polyphenol compound containing a large number of biphenyl pyrogallol and catechol groups. It not only has excellent antioxidant and anti-aging properties, but also can form a physical cross-linked network structure with polymers through interactions such as hydrogen bonding and π-π stacking, which tightly attaches grape seed, Bletilla striata and coconut water into the hydrogel, improving utilization and moisturizing effect.

[0023] More preferably, in step (2), the ratio of grape seed polyphenol extract, coconut water, tannic acid, allantoin skin care agent, and hyaluronic acid hydrogel is (10-50) mL:(10-30) mL:(0.05-0.2) g:(0.01-0.1) g:1 g.

[0024] (III) Beneficial Technical Effects

[0025] This invention uses grape seed powder and Bletilla striata powder as raw materials. A flash extraction process is used to extract a grape seed and Bletilla striata extract. This extract is then added to a hyaluronic acid hydrogel along with coconut water and tannic acid, followed by swelling, drying, grinding, and sieving to obtain a modified hydrogel powder. Polylactic acid (PLA) nanofiber membranes are prepared using solution spinning, followed by surface plasma treatment to obtain amino-modified PLA nanofiber membranes. Glutaraldehyde is used to treat the nanofiber membranes, introducing aldehyde groups onto the surface, and spermidine is grafted onto the membrane to obtain spermidine-modified PLA nanofibers. Finally, the modified hydrogel powder is added to deionized water, stirred and dispersed, and then the spermidine-modified PLA nanofiber membrane is immersed in the solution, thoroughly stirred and mixed, and then removed to obtain an antioxidant hydrogel-based face mask.

[0026] This invention uses a biodegradable polylactic acid nanofiber membrane as a substrate, and introduces spermidine onto its surface. This not only improves the hydrophilicity of the nanofiber membrane, but also allows the spermidine to adhere firmly to the surface of the fiber membrane, preventing migration. Since spermidine itself has antioxidant, anti-aging, and life-extending effects, the mask prepared from it also exhibits good anti-aging and antioxidant properties. The modified hydrogel powder prepared by this invention contains antioxidant and anti-aging substances such as grape seed extract, Bletilla striata extract, coconut water, and tannins, which work synergistically to further enhance the antioxidant effect of the mask.

[0027] This invention combines polylactic acid nanofiber membranes with poor hydrophilicity with modified hydrogels, which improves the adhesion, moisturizing properties and high water retention capacity of the antioxidant hydrogel-based mask. It is also biodegradable, mild and non-irritating. In addition, the raw materials used in this invention are simple and readily available, and safe to use. Detailed Implementation

[0028] The present invention will be further described in detail below with reference to the embodiments. However, it should be understood that these embodiments and comparative examples are merely for illustrating the present invention and should not be construed as limiting the scope of the appended claims in any way.

[0029] Example 1

[0030] (1) Place 1g of grape seed powder and 1g of Bletilla striata powder in a container, add 20mL of 50% ethanol aqueous solution, stir and disperse, place in a flash extraction device, and extract using flash extraction technology, wherein the extraction voltage is 100V, the number of extractions is 3, the extraction time is 40s, after extraction is completed, separate and filter to obtain grape seed Bletilla striata extract.

[0031] (2) Add 20 mL of grape seed extract, 20 mL of coconut water, 0.1 g of tannic acid, and 0.02 g of allantoin skin care agent to 2 g of hyaluronic acid hydrogel. Under room temperature conditions, swell and shake for 24 h, remove, wash with deionized water, dry, grind and sieve to obtain modified hydrogel powder.

[0032] (3) Add 1g of polylactic acid to 10mL of 5% ethanol-dichloromethane solution, stir to dissolve, and prepare polylactic acid nanofiber membrane by solution spray spinning method, wherein the gas flow pressure is 0.2MPa, the receiving distance is 20cm, the nozzle diameter is 0.5mm, dry, and then place it in the cavity of the plasma surface active agent for surface plasma treatment. The control conditions are: under ammonia conditions, treat with 50W power for 30s to obtain amino-modified polylactic acid nanofiber membrane.

[0033] (4) The amino-modified polylactic acid nanofiber membrane was immersed in an 8% glutaraldehyde aqueous solution and reacted at 35°C for 3 hours. After washing with deionized water and drying, a 5% spermidine aqueous solution was added and the membrane was soaked for 8 hours. After the reaction was completed, the membrane was washed with deionized water and dried to obtain the spermidine-modified polylactic acid nanofiber membrane.

[0034] (5) Add the modified hydrogel powder to deionized water, stir and disperse to prepare a 5% solution, then immerse the spermidine-modified polylactic acid nanofiber membrane in it, stir and mix thoroughly, and take it out to obtain an antioxidant hydrogel base mask.

[0035] Example 2

[0036] (1) Place 1g of grape seed powder and 1g of Bletilla striata powder in a container, add 20mL of 40% ethanol aqueous solution, stir and disperse, place in a flash extraction device, and extract using flash extraction technology, wherein the extraction voltage is 150V, the number of extractions is 2, the extraction time is 50s, after extraction is completed, separate and filter to obtain grape seed Bletilla striata extract.

[0037] (2) Add 40 mL of grape seed extract, 30 mL of coconut water, 0.2 g of tannic acid, and 0.05 g of allantoin skin care agent to 2 g of hyaluronic acid hydrogel. Under room temperature conditions, swell and shake for 24 h, remove, wash with deionized water, dry, grind and sieve to obtain modified hydrogel powder.

[0038] (3) Add 1g of polylactic acid to 10mL of 5% ethanol-dichloromethane solution, stir to dissolve, and prepare polylactic acid nanofiber membrane by solution spray spinning method, wherein the gas flow pressure is 0.2MPa, the receiving distance is 20cm, the nozzle diameter is 0.5mm, dry, and then place it in the cavity of the plasma surface active agent for surface plasma treatment. The control conditions are: under ammonia conditions, treat with 50W power for 30s to obtain amino-modified polylactic acid nanofiber membrane.

[0039] (4) The amino-modified polylactic acid nanofiber membrane was immersed in a 6% glutaraldehyde aqueous solution and reacted at 35°C for 3 hours. After washing with deionized water and drying, a 5% spermidine aqueous solution was added and the membrane was soaked for 5 hours. After the reaction was completed, the membrane was washed with deionized water and dried to obtain the spermidine-modified polylactic acid nanofiber membrane.

[0040] (5) Add the modified hydrogel powder to deionized water, stir and disperse to prepare an 8% solution, then immerse the spermidine-modified polylactic acid nanofiber membrane in it, stir and mix thoroughly, and take it out to obtain an antioxidant hydrogel base mask.

[0041] Example 3

[0042] (1) Place 1g of grape seed powder and 1g of Bletilla striata powder in a container, add 20mL of 50% ethanol aqueous solution, stir and disperse, place in a flash extraction device, and extract using flash extraction technology, wherein the extraction voltage is 120V, the number of extractions is 4, the extraction time is 60s, after extraction is completed, separate and filter to obtain grape seed Bletilla striata extract.

[0043] (2) Add 60 mL of grape seed extract, 40 mL of coconut water, 0.3 g of tannic acid, and 0.1 g of allantoin skin care agent to 2 g of hyaluronic acid hydrogel. Under room temperature conditions, swell and shake for 24 h, remove, wash with deionized water, dry, grind and sieve to obtain modified hydrogel powder.

[0044] (3) Add 1g of polylactic acid to 10mL of 5% ethanol-dichloromethane solution, stir to dissolve, and prepare polylactic acid nanofiber membrane by solution spray spinning method, wherein the gas flow pressure is 0.2MPa, the receiving distance is 20cm, the nozzle diameter is 0.5mm, dry, and then place it in the cavity of the plasma surface active agent for surface plasma treatment. The control conditions are: under ammonia conditions, treat with 50W power for 30s to obtain amino-modified polylactic acid nanofiber membrane.

[0045] (4) The amino-modified polylactic acid nanofiber membrane was immersed in a 10% glutaraldehyde aqueous solution and reacted at 30°C for 2 hours. After washing with deionized water and drying, a 4% spermidine aqueous solution was added and the membrane was soaked for 5 hours. After the reaction was completed, the membrane was washed with deionized water and dried to obtain the spermidine-modified polylactic acid nanofiber membrane.

[0046] (5) Add the modified hydrogel powder to deionized water, stir and disperse to prepare a 10% solution, then immerse the spermidine-modified polylactic acid nanofiber membrane in it, stir and mix thoroughly, and take it out to obtain an antioxidant hydrogel base mask.

[0047] Example 4

[0048] (1) Place 1g of grape seed powder and 1g of Bletilla striata powder in a container, add 20mL of 60% ethanol aqueous solution, stir and disperse, place in a flash extraction device, and extract using flash extraction technology, wherein the extraction voltage is 120V, the number of extractions is 4, the extraction time is 30s, after extraction is completed, separate and filter to obtain grape seed Bletilla striata extract.

[0049] (2) Add 80 mL of grape seed extract, 50 mL of coconut water, 0.4 g of tannic acid, and 0.15 g of allantoin skin care agent to 2 g of hyaluronic acid hydrogel. Under room temperature conditions, swell and shake for 24 h, remove, wash with deionized water, dry, grind and sieve to obtain modified hydrogel powder.

[0050] (3) Add 1g of polylactic acid to 10mL of 5% ethanol-dichloromethane solution, stir to dissolve, and prepare polylactic acid nanofiber membrane by solution spray spinning method, wherein the gas flow pressure is 0.2MPa, the receiving distance is 20cm, the nozzle diameter is 0.5mm, dry, and then place it in the cavity of the plasma surface active agent for surface plasma treatment. The control conditions are: under ammonia conditions, treat with 50W power for 30s to obtain amino-modified polylactic acid nanofiber membrane.

[0051] (4) The amino-modified polylactic acid nanofiber membrane was immersed in a 5% glutaraldehyde aqueous solution and reacted at 30°C for 4 hours. After washing with deionized water and drying, a 2% spermidine aqueous solution was added and the membrane was soaked for 12 hours. After the reaction was completed, the membrane was washed with deionized water and dried to obtain the spermidine-modified polylactic acid nanofiber membrane.

[0052] (5) Add the modified hydrogel powder to deionized water, stir and disperse to prepare a 12% solution, then immerse the spermidine-modified polylactic acid nanofiber membrane in it, stir and mix thoroughly, take it out, and obtain an antioxidant hydrogel base mask.

[0053] Example 5

[0054] (1) Place 1g of grape seed powder and 1g of Bletilla striata powder in a container, add 20mL of 45% ethanol aqueous solution, stir and disperse, place in a flash extraction device, and extract using flash extraction technology, wherein the extraction voltage is 150V, the number of extractions is 2, the extraction time is 40s, after extraction is completed, separate and filter to obtain grape seed Bletilla striata extract.

[0055] (2) Add 100 mL of grape seed extract, 60 mL of coconut water, 0.4 g of tannic acid, and 0.2 g of allantoin skin care agent to 2 g of hyaluronic acid hydrogel. Under room temperature conditions, swell and shake for 24 h, remove, wash with deionized water, dry, grind and sieve to obtain modified hydrogel powder.

[0056] (3) Add 1g of polylactic acid to 10mL of 5% ethanol-dichloromethane solution, stir to dissolve, and prepare polylactic acid nanofiber membrane by solution spray spinning method, wherein the gas flow pressure is 0.2MPa, the receiving distance is 20cm, the nozzle diameter is 0.5mm, dry, and then place it in the cavity of the plasma surface active agent for surface plasma treatment. The control conditions are: under ammonia conditions, treat with 50W power for 30s to obtain amino-modified polylactic acid nanofiber membrane.

[0057] (4) The amino-modified polylactic acid nanofiber membrane was immersed in an 8% glutaraldehyde aqueous solution and reacted at 35°C for 3 hours. After washing with deionized water and drying, a 5% spermidine aqueous solution was added and the membrane was soaked for 6 hours. After the reaction was completed, the membrane was washed with deionized water and dried to obtain the spermidine-modified polylactic acid nanofiber membrane.

[0058] (5) Add the modified hydrogel powder to deionized water, stir and disperse to prepare a 15% solution, then immerse the spermidine-modified polylactic acid nanofiber membrane in it, stir and mix thoroughly, and take it out to obtain an antioxidant hydrogel base mask.

[0059] Comparative Example 1

[0060] The difference between this comparative example and Example 1 is that polylactic acid nanofiber membrane is used instead of spermidine-modified polylactic acid nanofiber membrane.

[0061] Moisturizing performance test: At 25℃, a layer of medical breathable tape was flatly attached to a glass slide, and the mask was placed on the glass slide. The mass M1 was weighed and dried in a desiccator with a relative humidity of 50% for 12 hours. The weight M2 was then weighed and the moisturizing rate was calculated. Moisturizing rate (%) = M2 / M1 × 100%.

[0062] Table 1:

[0063]

[0064]

[0065] As can be seen from the table, the facial mask prepared by this invention has a good moisturizing effect.

[0066] Irritation test: 100 volunteers were selected, including 50 men and 50 women, aged 20-35 years, with healthy skin. The mask was placed on the back of the volunteer's hand, with the other hand as a control. The mask was left on for 15 minutes, and then washed off. The skin changes on the sample area were observed. The test was conducted continuously for one week.

[0067] Table 2:

[0068] Skin changes Example 1 No skin redness, itching, allergies, or other abnormal symptoms. Example 2 No skin redness, itching, allergies, or other abnormal symptoms. Example 3 No skin redness, itching, allergies, or other abnormal symptoms. Example 4 No skin redness, itching, allergies, or other abnormal symptoms. Example 5 No skin redness, itching, allergies, or other abnormal symptoms. Comparative Example 1 No skin redness, itching, allergies, or other abnormal symptoms.

[0069] As can be seen from the table, the face mask prepared by this invention is non-irritating.

[0070] Antioxidant performance test: Accurately weigh 0.039g DPPH, make up to 50mL with 95% ethanol, then dilute 10 times to obtain 0.6mmol / L DPPH, take 10mL and add it to the mask, incubate in the dark for 30min, take 2mL and measure the optical density at 517nm. Use deionized water instead of the mask as a negative control group. DPPH free radical scavenging efficiency (%) = [1-(experimental group optical density value / control group optical density value)]×100%.

[0071] Table 3:

[0072]

[0073]

[0074] As shown in the table, the facial mask prepared by this invention has good antioxidant and anti-aging properties.

[0075] The technical solutions of the above embodiments are preferred embodiments of the present invention. Several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered to be within the protection scope of the present invention.

Claims

1. A method of preparing an antioxidant hydrogel-based facial mask, characterized by, The preparation method of the antioxidant hydrogel-based facial mask is: The modified hydrogel powder is added into deionized water, stirred and dispersed to prepare a 5-15% solution, and then the spermidine-modified polylactic acid nanofiber membrane is immersed in the solution, stirred evenly, taken out, and the antioxidant hydrogel-based facial mask is obtained; The preparation method of the modified hydrogel powder is: (1) The grape seed powder and white peony powder are placed in a container, and an ethanol aqueous solution is added and stirred and dispersed, and then the mixture is placed in a flash extraction device and extracted by a flash extraction process. After extraction, the mixture is separated and filtered to obtain grape seed and white peony extract; (2) The grape seed and white peony extract, coconut water, tannic acid, and allantoin skin care agent are added to the hyaluronic acid hydrogel, which is swelled and shaken at room temperature for 24 h, taken out, washed with deionized water, dried, ground and sieved to obtain the modified hydrogel powder.

2. The method for preparing the antioxidant hydrogel-based face mask according to claim 1, characterized in that, In the (1), the flash extraction process is as follows: the extraction voltage is 100-150 V, the extraction times is 2-4 times, and the extraction time is 30-60 s.

3. The method of claim 1, wherein the antioxidant hydrogel-based facial mask is prepared by mixing the antioxidant hydrogel base and the antioxidant facial mask additive. In the (1), the mass fraction of the ethanol aqueous solution is 40-60%.

4. The method of claim 1, wherein the antioxidant hydrogel-based facial mask is prepared by mixing the antioxidant hydrogel base and the antioxidant facial mask additive. In the (2), the amount ratio of the grape seed and white peony extract, coconut water, tannic acid, allantoin skin care agent, and hyaluronic acid hydrogel is (10-50) mL:(10-30) mL:(0.05-0.2) g:(0.01-0.1) g:1 g.

5. The method of claim 1, wherein the antioxidant hydrogel-based facial mask is prepared by mixing the antioxidant hydrogel-based facial mask composition with water. The preparation method of the spermidine-modified polylactic acid nanofiber membrane is: S1, polylactic acid is added to a 5% mass fraction ethanol dichloromethane solution, stirred and dissolved, and a polylactic acid nanofiber membrane is prepared by solution electrospinning, dried, and then placed in the cavity of a plasma surface activation instrument for surface plasma treatment to obtain an amino-modified polylactic acid nanofiber membrane; S2, the amino-modified polylactic acid nanofiber membrane is immersed in a glutaraldehyde aqueous solution at 30-35°C for 2-4 h, washed with deionized water, dried, and then a 2-5% mass fraction spermidine aqueous solution is added and soaked for 5-12 h. After the reaction is completed, the membrane is washed with deionized water and dried to obtain a spermidine-modified polylactic acid nanofiber membrane.

6. The method of claim 5, wherein the antioxidant hydrogel-based facial mask is prepared by mixing the antioxidant hydrogel-based facial mask composition with water. In the S1, the air flow pressure in the solution electrospinning is 0.2 MPa, the receiving distance is 20 cm, and the nozzle diameter is 0.5 mm.

7. The method of claim 5, wherein the antioxidant hydrogel-based facial mask is prepared by mixing the antioxidant hydrogel-based facial mask composition with water. In the S1, the control conditions of the plasma surface activation instrument are as follows: the instrument is operated under ammonia gas at a power of 50 W for 30 s.

8. The method of claim 5, wherein the antioxidant hydrogel-based facial mask is prepared by mixing the antioxidant hydrogel-based facial mask composition with water. In the S2, the mass fraction of the glutaraldehyde aqueous solution is 5-10%.

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