Preparation method of antioxidant hydrogel-based mask

Abstract

The invention relates to the technical field of masks, and discloses a preparation method of an antioxidant hydrogel-based mask, which comprises the following steps: adding a bletilla striata extract, coconut water, tannic acid and the like into hyaluronic acid hydrogel, swelling, drying, grinding and sieving to obtain modified hydrogel powder; the preparation method comprises the following steps: by taking polylactic acid as a raw material, carrying out surface plasma treatment on the polylactic acid through a solution jet spinning method to obtain an amino modified polylactic acid nanofiber membrane, treating the nanofiber membrane with glutaraldehyde, introducing an aldehyde group on the surface of the nanofiber membrane, and grafting spermidine to obtain the spermidine modified polylactic acid nanofiber. And finally, adding the modified hydrogel powder into deionized water, stirring and dispersing, immersing the spermidine modified polylactic acid nanofiber membrane into the solution, fully stirring and uniformly mixing, and taking out to obtain the antioxidant hydrogel-based mask. The hydrogel-based mask prepared by the preparation method disclosed by the invention has relatively good oxidation resistance and moisturizing performance.

Description

Technical Field

[0001] The invention relates to the technical field of facial masks, and in particular to a method for preparing an antioxidant hydrogel-based facial mask. Background Art

[0002] With the rapid development of the national economy, people pay more and more attention to self-care, among which facial mask products have become an indispensable and important part. Nanofiber membranes are widely used in the field of daily necessities due to their advantages of high porosity, large surface area, and controllable morphology. However, nanofiber membranes have problems such as poor moisturizing and poor adhesion. Therefore, it is necessary to improve the moisturizing and adhesion of nanofiber membranes to expand the field. Hydrogel is a polymer material with a three-dimensional cross-linked structure, which has a high water content, good moisturizing, biocompatibility and functionality, but traditional hydrogels have poor biocompatibility.

[0003] Polylactic acid is a biodegradable polymer material, which is widely used in the fields of biomedicine and materials, etc. However, it has high crystallinity, no active reactive groups, poor hydrophilicity, and weak adhesion to cells. Therefore, its application range is greatly limited, and the hydrophilic properties of the polylactic acid nanofiber membrane prepared from polylactic acid are also poor. Summary of the invention

[0004] 1. Technical issues to be resolved

[0005] In view of the deficiencies in the prior art, the present invention provides a method for preparing an antioxidant hydrogel-based facial mask, in which a modified polylactic acid nanofiber membrane is compounded with a modified hydrogel to integrate the advantages of both and prepare a moisturizing and antioxidant facial mask.

[0006] (II) Technical solution

[0007] A method for preparing an antioxidant hydrogel-based facial mask, the method for preparing the antioxidant hydrogel-based facial mask comprising:

[0008] 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 therein, stirred and mixed thoroughly, and taken out to obtain an antioxidant hydrogel-based facial mask.

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

[0010] S1, adding polylactic acid to a 5% by mass ethanol dichloromethane solution, stirring to dissolve, preparing a polylactic acid nanofiber membrane by a solution spinning method, drying, and then placing it in the cavity of a plasma surfactant instrument for surface plasma treatment to obtain an amino-modified polylactic acid nanofiber membrane;

[0011] S2. Immerse the amino-modified polylactic acid nanofiber membrane in a glutaraldehyde aqueous solution, react at 30-35°C for 2-4 hours, wash with deionized water, and dry. Then add a 2-5% by mass spermidine aqueous solution and soak for reaction for 5-12 hours. After the reaction is completed, wash with deionized water and dry to obtain a spermidine-modified polylactic acid nanofiber membrane.

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

[0013] Further preferably, in S1, the control condition of the plasma surfactant instrument is to treat at a power of 50 W for 30 seconds under ammonia conditions.

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

[0015] Preferably, the preparation method of the modified hydrogel powder is

[0016] (1) placing grape seed powder and bletilla striata powder in a container, adding 40-60% ethanol aqueous solution thereto, stirring and dispersing, placing in a flash extraction device, extracting by a flash extraction process, and after the extraction is completed, separating and filtering to obtain a grape seed bletilla striata extract, the flash extraction process is: extraction voltage is 100-150V, extraction times are 2-4 times, and extraction time is 30-60s;

[0017] (2) adding grape seed bletilla extract, coconut water, tannic acid, and allantoin skin care agent to the hyaluronic acid hydrogel, swelling and shaking for 24 hours at room temperature, taking out, washing with deionized water, drying, grinding and sieving to obtain a modified hydrogel powder;

[0018] The grape seeds, white radix and coconut water are all commercially available;

[0019] The grape seeds are rich in polyphenols, flavonoids and other active substances. As a natural and efficient antioxidant, they can remove active oxygen produced by oxidative stress. They are extracted using a flash extraction process and added to a facial mask to enhance the antioxidant and anti-aging effects of the mask.

[0020] The Bletilla striata is a traditional Chinese medicine, which contains Bletilla striata polysaccharide. Bletilla striata polysaccharide has a good scavenging effect on hydroxyl free radicals and superoxide anion free radicals. It is extracted using a flash extraction process and added to a facial mask to enhance the mask's antioxidant and anti-aging effects.

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

[0022] The tannic acid is a natural water-soluble polyphenol compound containing a large amount of 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 bonds and π-π stacking, tightly attaching grape seeds, white ginseng, and coconut water to the inside of the hydrogel, thereby improving utilization and moisturizing effects.

[0023] Further preferably, in (2), the usage 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] The present invention uses grape seed powder and bletilla striata powder as raw materials, uses flash extraction process, extracts and obtains grape seed bletilla striata extract, then adds it to hyaluronic acid hydrogel with coconut water, tannic acid, etc., swells, is dried, and is ground and sieved to obtain modified hydrogel powder. Using polylactic acid as raw material, polylactic acid nanofiber film is prepared using solution jet spinning method, then surface plasma treatment is performed to it, amino-modified polylactic acid nanofiber film is obtained, glutaraldehyde is used to process nanofiber film, aldehyde group is introduced on the fiber film surface, spermidine is grafted, and spermidine modified polylactic acid nanofiber is obtained. Finally, modified hydrogel powder is added to deionized water, stirred and dispersed, then spermidine modified polylactic acid nanofiber film is immersed therein, fully stirred and mixed, taken out, and antioxidant hydrogel-based facial mask is obtained.

[0026] The present invention uses biodegradable polylactic acid nanofiber membrane as a substrate, and introduces spermidine on the surface thereof, which can not only improve the hydrophilicity of the nanofiber membrane, but also spermidine can firmly adhere to the surface of the fiber membrane and is not easy to migrate out. Since spermidine itself has the effects of anti-oxidation, anti-aging, and life extension, the facial mask prepared by it also has good anti-aging and anti-oxidation effects. The modified hydrogel powder prepared by the present invention contains antioxidant and anti-aging substances such as grape seeds, white schizonepeta, coconut water, and tannic acid, which work synergistically to further improve the antioxidant effect of the facial mask.

[0027] The present invention compounds a polylactic acid nanofiber membrane with poor hydrophilicity with a modified hydrogel, thereby improving the fit, moisturizing properties and high water retention capacity of the antioxidant hydrogel-based facial mask, and has the characteristics of biodegradability, mildness and non-irritation. In addition, the raw materials used in the present invention are simple and easy to obtain, and safe to use. DETAILED DESCRIPTION

[0028] The present invention is further described in detail below in conjunction with the examples. However, it should be understood that these examples and comparative examples are only used to specifically illustrate the present invention and should not be understood as limiting the scope of the appended claims of the present invention in any form.

[0029] Example 1

[0030] (1) 1 g of grape seed powder and 1 g of Bletilla striata powder are placed in a container, 20 mL of 50% ethanol aqueous solution is added thereto, the mixture is stirred and dispersed, and the mixture is placed in a flash extraction device for extraction using a flash extraction process, wherein the extraction voltage is 100 V, the number of extractions is 3, and the extraction time is 40 s. After the extraction is completed, the mixture is separated and filtered to obtain a grape seed Bletilla striata extract.

[0031] (2) Add 20 mL of grape seed Bletilla striata 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, swell and shake at room temperature for 24 h, take out, wash with deionized water, dry, grind and sieve to obtain modified hydrogel powder.

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

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

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

[0035] Example 2

[0036] (1) 1 g of grape seed powder and 1 g of Bletilla striata powder are placed in a container, 20 mL of 40% ethanol aqueous solution is added thereto, the mixture is stirred and dispersed, and the mixture is placed in a flash extraction device for extraction using a flash extraction process, wherein the extraction voltage is 150 V, the number of extractions is 2, and the extraction time is 50 s. After the extraction is completed, the mixture is separated and filtered to obtain a grape seed Bletilla striata extract.

[0037] (2) 40 mL of grape seed Bletilla striata extract, 30 mL of coconut water, 0.2 g of tannic acid, and 0.05 g of allantoin skin care agent were added to 2 g of hyaluronic acid hydrogel, and the mixture was swollen and shaken at room temperature for 24 h. The mixture was taken out, washed with deionized water, dried, ground and sieved to obtain a modified hydrogel powder.

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

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

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

[0041] Example 3

[0042] (1) 1 g of grape seed powder and 1 g of Bletilla striata powder are placed in a container, 20 mL of 50% ethanol aqueous solution is added thereto, the mixture is stirred and dispersed, and the mixture is placed in a flash extraction device for extraction using a flash extraction process, wherein the extraction voltage is 120 V, the number of extractions is 4, and the extraction time is 60 s. After the extraction is completed, the mixture is separated and filtered to obtain a grape seed Bletilla striata extract.

[0043] (2) 60 mL of grape seed Bletilla striata extract, 40 mL of coconut water, 0.3 g of tannic acid, and 0.1 g of allantoin skin care agent were added to 2 g of hyaluronic acid hydrogel, and the mixture was swollen and shaken at room temperature for 24 h. The mixture was taken out, washed with deionized water, dried, ground and sieved to obtain a modified hydrogel powder.

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

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

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

[0047] Example 4

[0048] (1) 1 g of grape seed powder and 1 g of Bletilla striata powder are placed in a container, 20 mL of 60% ethanol aqueous solution is added thereto, the mixture is stirred and dispersed, and the mixture is placed in a flash extraction device for extraction using a flash extraction process, wherein the extraction voltage is 120 V, the number of extractions is 4, and the extraction time is 30 s. After the extraction is completed, the mixture is separated and filtered to obtain a grape seed Bletilla striata extract.

[0049] (2) 80 mL of grape seed Bletilla striata extract, 50 mL of coconut water, 0.4 g of tannic acid, and 0.15 g of allantoin skin care agent were added to 2 g of hyaluronic acid hydrogel, and the mixture was swollen and shaken at room temperature for 24 h. The mixture was taken out, washed with deionized water, dried, ground and sieved to obtain a modified hydrogel powder.

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

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

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

[0053] Example 5

[0054] (1) 1 g of grape seed powder and 1 g of Bletilla striata powder are placed in a container, 20 mL of 45% ethanol aqueous solution is added thereto, the mixture is stirred and dispersed, and the mixture is placed in a flash extraction device for extraction using a flash extraction process, wherein the extraction voltage is 150 V, the number of extractions is 2, and the extraction time is 40 s. After the extraction is completed, the mixture is separated and filtered to obtain a grape seed Bletilla striata extract.

[0055] (2) 100 mL of grape seed Bletilla striata extract, 60 mL of coconut water, 0.4 g of tannic acid, and 0.2 g of allantoin skin care agent were added to 2 g of hyaluronic acid hydrogel, and the mixture was swollen and shaken at room temperature for 24 h. The mixture was taken out, washed with deionized water, dried, ground and sieved to obtain a modified hydrogel powder.

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

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

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

[0059] Comparative Example 1

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

[0061] Moisturizing performance test: At 25°C, stick a layer of medical breathable tape flatly on a glass sheet, take the mask and place it on the glass sheet, weigh the mass M1, dry it in a dryer with a relative humidity of 50% for 12 hours, weigh M2, and calculate the moisturizing rate. Moisturizing rate (%) = M2 / M1×100%.

[0062] Table 1:

[0063]

[0064]

[0065] It can be seen from the table that the facial mask prepared by the present invention has a good moisturizing effect.

[0066] Irritation test: 100 volunteers were selected, including 50 men and 50 women, aged between 20 and 35 years old, with healthy skin. The mask was placed on the back of the volunteers' hands, and the other back of the hand was used as a control. The mask was left on for 15 minutes, then washed after 15 minutes, and the skin changes of the sample skin area were observed. The test was carried out continuously for 1 week.

[0067] Table 2:

[0068] Skin changes Example 1 No abnormal skin phenomena such as redness, itching, allergies, etc. Example 2 No abnormal skin phenomena such as redness, itching, allergies, etc. Example 3 No abnormal skin phenomena such as redness, itching, allergies, etc. Example 4 No abnormal skin phenomena such as redness, itching, allergies, etc. Example 5 No abnormal skin phenomena such as redness, itching, allergies, etc. Comparative Example 1 No abnormal skin phenomena such as redness, itching, allergies, etc.

[0069] It can be seen from the table that the facial mask prepared by the present invention is non-irritating.

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

[0071] Table 3:

[0072]

[0073]

[0074] It can be seen from the table that the facial mask prepared by the present invention has good anti-oxidation and anti-aging properties.

[0075] The technical solutions of the above embodiments are preferred implementation modes of the present invention. Several improvements and changes may be made without departing from the principles of the present invention. These improvements and changes should also be regarded as within the protection scope of the present invention.

Claims

1. A method for preparing an antioxidant hydrogel-based facial mask, characterized in that: The preparation method of the antioxidant hydrogel-based facial mask is as follows: 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 therein, stirred and mixed thoroughly, and taken out to obtain an antioxidant hydrogel-based facial mask.

2. The method for preparing the antioxidant hydrogel-based facial mask according to claim 1, characterized in that: The preparation method of the modified hydrogel powder is as follows: (1) placing grape seed powder and Bletilla striata powder in a container, adding ethanol aqueous solution thereto, stirring and dispersing, placing in a flash extraction device, extracting by a flash extraction process, and after the extraction is completed, separating and filtering to obtain a grape seed and Bletilla striata extract; (2) Add grape seed bletilla extract, coconut water, tannic acid, and allantoin skin care agent to the hyaluronic acid hydrogel, swell and shake at room temperature for 24 hours, take out, wash with deionized water, dry, grind and sieve to obtain modified hydrogel powder.

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

4. The method for preparing the antioxidant hydrogel-based facial mask according to claim 2, characterized in that: In the above (1), the mass fraction of the ethanol aqueous solution is 40-60%.

5. The method for preparing the antioxidant hydrogel-based facial mask according to claim 2, characterized in that: In the above (2), the usage 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.

6. The method for preparing the antioxidant hydrogel-based facial mask according to claim 1, characterized in that: The preparation method of the spermidine modified polylactic acid nanofiber membrane is: S1, adding polylactic acid to a 5% by mass ethanol dichloromethane solution, stirring to dissolve, preparing a polylactic acid nanofiber membrane by a solution spinning method, drying, and then placing it in the cavity of a plasma surfactant instrument for surface plasma treatment to obtain an amino-modified polylactic acid nanofiber membrane; S2. Immerse the amino-modified polylactic acid nanofiber membrane in a glutaraldehyde aqueous solution, react at 30-35°C for 2-4 hours, wash with deionized water, and dry. Then add a 2-5% by mass spermidine aqueous solution and soak for reaction for 5-12 hours. After the reaction is completed, wash with deionized water and dry to obtain a spermidine-modified polylactic acid nanofiber membrane.

7. The method for preparing the antioxidant hydrogel-based facial mask according to claim 6, characterized in that: In the S1, the air flow pressure in the solution jet spinning method is 0.2 MPa, the receiving distance is 20 cm, and the nozzle diameter is 0.5 mm.

8. The method for preparing the antioxidant hydrogel-based facial mask according to claim 6, characterized in that: In S1, the control condition of the plasma surfactant instrument is to treat at a power of 50 W for 30 seconds under ammonia conditions.

9. The method for preparing the antioxidant hydrogel-based facial mask according to claim 6, characterized in that: In the S2, the mass fraction of the glutaraldehyde aqueous solution is 5-10%.

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