CN114469776B - Electrostatic spinning mask and preparation method thereof - Google Patents

Electrostatic spinning mask and preparation method thereof Download PDF

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Publication number
CN114469776B
CN114469776B CN202111612387.2A CN202111612387A CN114469776B CN 114469776 B CN114469776 B CN 114469776B CN 202111612387 A CN202111612387 A CN 202111612387A CN 114469776 B CN114469776 B CN 114469776B
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electrostatic spinning
mask
spinning
schizophyllan
hydrolyzed silk
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CN114469776A (en
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郭朝万
胡露
孙怀庆
聂艳峰
江川霞
蒲艳
陈杰
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Guangdong Marubi Biological Technology Co Ltd
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Guangdong Marubi Biological Technology Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0212Face masks
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/64Proteins; Peptides; Derivatives or degradation products thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0092Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Engineering & Computer Science (AREA)
  • Epidemiology (AREA)
  • Birds (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Dermatology (AREA)
  • Gerontology & Geriatric Medicine (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Cosmetics (AREA)

Abstract

The invention provides an electrostatic spinning mask and a preparation method thereof. The electrostatic spinning facial mask comprises an electrostatic spinning fiber membrane formed by schizophyllan and hydrolyzed silk. The facial mask is prepared by the aid of the schizophyllan and the hydrolyzed silk through electrostatic spinning, other auxiliaries are not needed, the schizophyllan and the hydrolyzed silk are matched with each other and have a synergistic effect, and when the facial mask is in contact with wet skin, the nano fibers are rapidly dissolved or gradually dissolved in the skin, so that an improved treatment effect is achieved, and water replenishing, wrinkle fading, skin elasticity increasing and aging delaying are further improved.

Description

Electrostatic spinning mask and preparation method thereof
Technical Field
The invention belongs to the field of cosmetics, and particularly relates to an electrostatic spinning mask and a preparation method thereof.
Background
The mask is one of the most widely used personal care products, and has the effects of softening the stratum corneum, preventing water evaporation, accelerating the osmotic absorption of nutrients and the like. The traditional mask has complex formula components and needs a plurality of unexpected auxiliary agents of the functional components, and the auxiliary agents bring a large burden to the skin and can even cause allergy to users of certain sensitive skins. At present, in the cosmetic market, products related to the electrostatic spinning facial mask have been developed, however, the products need to be supported by a non-woven fabric as a base material, and the functional components of the products are easily absorbed by the non-woven fabric when the products are used. In addition, the transdermal absorption capacity of the active substance in the facial mask is uncertain, and the active substance which is relatively active has the defects of easy variability and difficult storage.
CN109568173A discloses a collagen nano instant facial mask using hyaluronic acid as a skeleton and a preparation method thereof, the facial mask comprises a non-woven fabric substrate layer and a nanofiber layer, wherein the nanofiber layer is formed on the non-woven fabric substrate layer by adopting an electrostatic spinning method, and the nanofiber layer comprises: 10-35 parts of sodium hyaluronate, 6-50 parts of hydrolyzed collagen and 0.1-5 parts of surface active substances. The facial mask takes hyaluronic acid as a skeleton, but still needs to be formed on the non-woven fabric substrate layer for storage, and still needs to be additionally added with a surfactant, so that the component brings great burden to the skin and even can cause allergy to users with certain sensitive skin; in addition, although the mask has a certain moisturizing property, the anti-aging capability needs to be improved.
CN109674685A discloses a collagen nano instant facial mask using pullulanase as a framework and a preparation method thereof, the facial mask comprises a non-woven fabric base material layer and a nano fiber layer, wherein the nano fiber layer is formed on the non-woven fabric base material layer by adopting an electrostatic spinning method, and the nano fiber layer comprises: 10-60 parts of pullulanase polysaccharide and 5-40 parts of hydrolyzed collagen with lower molecular weight; and 0.1-5 parts by weight of a surface active substance. The mask takes pullulanase as a framework, but the pullulanase still needs to be formed on the non-woven fabric substrate layer to be stored in the same way, and a surfactant is still required to be additionally added, so that the component brings great burden to the skin and even can cause allergy to users with certain sensitive skin; in addition, although the mask has a certain moisturizing property, the anti-aging capability needs to be improved.
CN106551806A discloses a gradually dissolving moisture mask and a preparation method thereof. The method comprises the following steps: (1) Mixing the mixed aqueous solution of starch acetate and starch sugar with the aqueous solution of the moisturizing active ingredient or the mixed aqueous solution of the moisturizing active ingredient and disodium glycyrrhizinate, and uniformly dispersing to obtain a spinning solution; (2) And (4) carrying out electrostatic spinning on the spinning solution, and collecting by using a collecting device to obtain the gradually-dissolved moisturizing mask. The facial mask has certain moisturizing performance, but the anti-aging capability needs to be improved.
Therefore, the development of a cleaner and more efficient electrospun mask without the use of other additives is the focus of research in the field.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an electrostatic spinning mask and a preparation method thereof. The electrostatic spinning mask disclosed by the invention can be prepared by forming the active substance by a spinning process without using other auxiliaries, and is purer and more efficient.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides an electrospun facial mask comprising an electrospun fibrous membrane formed from a schizophyllan and hydrolyzed silk.
In the invention, the facial mask is prepared by the aid of the schizophyllan and the hydrolyzed silk through electrostatic spinning process, other auxiliary agents are not needed, the schizophyllan and the hydrolyzed silk are matched with each other and have a synergistic effect, and when the facial mask is contacted with wet skin, the nano fibers are rapidly dissolved or gradually dissolved in the skin, so that improved treatment effect is achieved, and water supplement, wrinkle lightening, skin elasticity increasing and aging delaying are further improved. Particularly, the skin nutrition metabolism is improved, the skin elasticity is kept, and meanwhile, the epidermal tissue is repaired, so that multiple effects of moisture preservation, wrinkle resistance and aging resistance are achieved.
The facial mask prepared by using the Schizophyllan as the main component has the advantages of large specific surface area, small fiber membrane pore diameter and high porosity, and has good effect on absorption and release of the Schizophyllan and hydrolyzed silk.
The HYDROLYZED SILK (HYDROLYZED SILK) is native macromolecular fibrin extracted from SILK, has content of 70-80% of SILK, and contains 18 amino groups. The invention uses the hydrolyzed silk as the main component to carry out electrostatic spinning, can replace the traditional silk non-woven fabric membrane, has the advantages of good skin-friendly property, biodegradability, soft and smooth touch, good air permeability, good moisture absorption and moisture release performance and the like, on the other hand, the electrostatic spinning membrane formed by electrostatic spinning has the advantages of small diameter of the hydrolyzed silk and three-dimensional porous structure, and the prepared facial mask has the advantages of large specific surface area, small pore diameter of the fiber membrane and high porosity, is more beneficial to directly acting on the skin, can be absorbed by the skin of a human body, can promote the secretion of collagen, and enhances the tension and elasticity of the skin.
Preferably, the mass ratio of the schizophyllan to the hydrolyzed silk is (0.1-10) to (5-30);
wherein "0.1 to 10" may be, for example, 0.1, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, etc.;
the "5 to 30" may be, for example, 5, 6, 7, 8, 9, 10, 12, 14, 16, 18, 20, 22, 24, 26, 28, 30, or the like.
Preferably, the mass ratio of the schizophyllan to the hydrolyzed silk is (5-10) to (15-20).
In the invention, the mass ratio of the schizophyllan to the hydrolyzed silk is preferably (5-10) to (15-20), multiple effects of moisturizing, anti-wrinkle and anti-aging are achieved within the range, if the schizophyllan is more and the hydrolyzed silk is less, the moisturizing performance is better, but the anti-wrinkle and anti-aging effects are poorer; if the quantity of schizophyllan is less and the quantity of hydrolyzed silk is more, the anti-wrinkle and anti-aging effects are better, but the water replenishing performance is poorer.
Preferably, the molecular weight of the schizophyllan is 100-1000kD, such as 100kD, 200kD, 300kD, 400kD, 500kD, 600kD, 700kD, 800kD, 900kD, 1000kD, etc., preferably 200-400kD.
Preferably, the raw materials for preparing the electrostatic spinning fiber membrane comprise the following components in percentage by mass: 0.1-10% (for example, 0.1%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, etc.) of schizophyllan and 5-30% (for example, 5%, 6%, 8%, 10%, 12%, 14%, 16%, 18%, 20%, 22%, 24%, 26%, 28%, 30%, etc.) of hydrolyzed silk, the balance being water.
In a second aspect, the present invention provides a method for preparing an electrospun facial mask as described in the first aspect, comprising the steps of:
(1) Mixing the schizophyllan, the hydrolyzed silk and water, and stirring to obtain a spinning solution;
(2) Injecting the spinning solution obtained in the step (1) in a high-voltage electric field, performing electrostatic spinning, and collecting by a collecting device to obtain the electrostatic spinning mask.
Preferably, in step (1), the rotation speed of the stirring is 1000-5000rpm, and may be, for example, 1000rpm, 1500rpm, 2000rpm, 2500rpm, 3000rpm, 3500rpm, 4000rpm, 4500rpm, 5000rpm, or the like.
Preferably, in step (1), the stirring temperature is 40-90 deg.C, such as 40 deg.C, 45 deg.C, 50 deg.C, 55 deg.C, 60 deg.C, 65 deg.C, 70 deg.C, 75 deg.C, 80 deg.C, 85 deg.C, 90 deg.C, etc., and the stirring time is 0.5-5h, such as 0.5h, 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h, etc.
Preferably, in the step (1), the specific preparation method of the spinning solution is as follows: the method comprises mixing the schizophyllan and water, stirring at 3000-5000rpm (such as 3000rpm, 3500rpm, 4000rpm, 4500rpm, 5000 rpm) and 50-90 deg.C (such as 50 deg.C, 55 deg.C, 60 deg.C, 65 deg.C, 70 deg.C, 75 deg.C, 80 deg.C, 85 deg.C, 90 deg.C) for 0.5-2h (such as 0.5h, 1h, 1.5h, 2h, etc.), adding hydrolyzed silk, and stirring at 1000-3000rpm (such as 1000rpm, 1500rpm, 2000rpm, 2500rpm, 3000 rpm) at 40-60 deg.C (such as 40 deg.C, 45 deg.C, 50 deg.C, 55 deg.C, 60 deg.C) for 0.5-3h (such as 0.5h, 1h, 1.5h, 2h, 2.5h, 3h, etc.) to obtain spinning solution.
Preferably, in the step (2), the specific parameters of the electrostatic spinning are as follows: the voltage is 15-25kV (for example, 15kV, 16kV, 18kV, 20kV, 22kV, 23kV, 25kV, etc.), the receiving distance is 10-20cm (for example, 10cm, 12cm, 14cm, 16cm, 18cm, 20cm, etc.), and the spinning rate is 0.1-1mL/h (for example, 0.1mL/h, 0.2mL/h, 0.4mL/h, 0.6mL/h, 0.8mL/h, 1mL/h, etc.).
Preferably, in step (2), the electrostatic spinning is performed with a needle diameter of 0.5-1mm, such as 0.5mm, 0.6mm, 0.7mm, 0.8mm, 0.9mm, 1mm, etc.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) Firstly, mixing schizophyllan and water, stirring for 1-2h at the rotating speed of 3000-5000rpm and the temperature of 70-90 ℃, adding hydrolyzed silk, and stirring for 1-2h at the rotating speed of 1000-3000rpm and the temperature of 50-60 ℃ to obtain a spinning solution;
(2) Performing electrostatic spinning on the spinning solution obtained in the step (1) to obtain the electrostatic spinning mask;
the specific parameters of the electrostatic spinning are as follows: the voltage is 15-25kV, the receiving distance is 10-20cm, and the spinning speed is 0.1-1mL/h; the field intensity of the low-voltage electrostatic field is 500-600V/m, and the sub-supercooling temperature is-20-0 ℃.
Compared with the prior art, the invention has the following beneficial effects:
(1) The electrostatic spinning mask can be prepared by forming the schizophyllan and the hydrolyzed silk by a spinning process, other auxiliaries are not needed, and the mask is purer and more efficient;
(2) The schizophyllan and the hydrolyzed silk are mutually matched, have a synergistic effect, and when the schizophyllan and the hydrolyzed silk are in contact with wet skin, the nano fibers are quickly dissolved or gradually dissolved in the skin so as to obtain an improved treatment effect, further improve water supplement, fade wrinkles, increase skin elasticity and delay aging.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitation of the present invention.
The following examples and comparative examples, where no specific techniques or conditions are indicated, can be performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or apparatus used are conventional products commercially available from a formal channel or may be prepared by the prior art, without reference to the manufacturer.
Example 1
The embodiment provides an electrostatic spinning mask, which is prepared by the following method:
(1) Mixing 7g of schizophyllan (with the average molecular weight of 300 kD) and 75g of deionized water, stirring at the rotating speed of 4000rpm for 1.5h at 80 ℃, adding 18g of hydrolyzed silk, and stirring at the rotating speed of 2000rpm for 1h at 60 ℃ to obtain a spinning solution;
(2) Performing electrostatic spinning on the spinning solution obtained in the step (1), and collecting the spinning solution through a collecting device to obtain the electrostatic spinning mask;
the specific parameters of the electrostatic spinning are as follows: the voltage is 15kV, the receiving distance is 15cm, the spinning speed is 0.2mL/h, and the diameter of a needle adopted by electrostatic spinning is 0.6mm.
Example 2
The embodiment provides an electrostatic spinning mask, which is prepared by the following method:
(1) Firstly, 5g of schizophyllan (with the average molecular weight of 400 kD) and 75g of deionized water are mixed, stirred for 0.5h at 90 ℃ at the rotating speed of 3000rpm, then 20g of hydrolyzed silk is added, and stirred for 3h at 60 ℃ at the rotating speed of 1000rpm to obtain a spinning solution;
(2) Performing electrostatic spinning on the spinning solution obtained in the step (1), and collecting the spinning solution through a collecting device to obtain the electrostatic spinning mask;
the specific parameters of the electrostatic spinning are as follows: the voltage is 20kV, the receiving distance is 10cm, the spinning speed is 0.1mL/h, and the diameter of a needle used for electrostatic spinning is 0.6mm.
Example 3
The embodiment provides an electrostatic spinning mask, which is prepared by the following method:
(1) Firstly, mixing 10g of schizophyllan (with the average molecular weight of 200 kD) and 75g of deionized water, stirring at the rotating speed of 5000rpm for 2h at 60 ℃, adding 15g of hydrolyzed silk, and stirring at the rotating speed of 3000rpm for 0.5h at 40 ℃ to obtain a spinning solution;
(2) Performing electrostatic spinning on the spinning solution obtained in the step (1), and collecting the spinning solution through a collecting device to obtain the electrostatic spinning mask;
the specific parameters of the electrostatic spinning are as follows: the voltage is 25kV, the receiving distance is 20cm, the spinning speed is 1mL/h, and the diameter of a needle used for electrostatic spinning is 0.6mm.
Example 4
The embodiment provides an electrostatic spinning mask, which is prepared by the following method:
(1) Firstly, mixing 10g of schizophyllan (with the average molecular weight of 200 kD) and 75g of deionized water, stirring at the rotating speed of 5000rpm for 2h at 60 ℃, adding 15g of hydrolyzed silk, and stirring at the rotating speed of 3000rpm for 0.5h at 40 ℃ to obtain a spinning solution;
(2) Performing electrostatic spinning on the spinning solution obtained in the step (1), and performing spinning on a silk spunlace non-woven fabric (the thickness of the spunlace non-woven fabric is 0.12 mm) through a spinning nozzle to form a film, so as to obtain the electrostatic spinning mask; the specific parameters of the electrostatic spinning are as follows: the voltage is 15kV, the receiving distance is 15cm, the spinning speed is 0.5mL/h, and the diameter of a needle adopted by electrostatic spinning is 0.6mm.
Example 5
This example provides an electrospun facial mask, which is different from example 1 only in that the amount of the schizophyllan added was 4g, and the amount of the hydrolyzed silk added was 21g.
Example 6
This example provides an electrospun facial mask, which differs from example 1 only in that the amount of the schizophyllan added was 20g and the amount of the hydrolyzed silk added was 5g.
Example 7
This example provides an electrospun mask, differing from example 1 only in that the average molecular weight of the schizophyllan was 100kD.
Example 8
This example provides an electrospun mask differing from example 1 only in that the average molecular weight of the schizophyllan was 1000kD.
Comparative example 1
The comparative example provides an electrospun facial mask prepared by the following method:
(1) Mixing 25g of hydrolyzed silk and 75g of deionized water, and stirring at the rotating speed of 2000rpm and the temperature of 60 ℃ for 3 hours to obtain a spinning solution;
(2) Performing electrostatic spinning on the spinning solution obtained in the step (1), and performing spinning on a silk spunlace non-woven fabric (the thickness of the spunlace non-woven fabric is 0.12 mm) through a spinning nozzle to form a film, so as to obtain the electrostatic spinning mask; the specific parameters of the electrostatic spinning are as follows: the voltage is 15kV, the receiving distance is 15cm, the spinning speed is 0.5mL/h, and the diameter of a needle used for electrostatic spinning is 0.6mm.
In this case, comparative example 1 had no addition of schizophyllan, which made it necessary to spray it onto the nonwoven substrate.
Comparative example 2
The comparative example provides an electrospun facial mask prepared by the following method:
(1) Mixing 25g of schizophyllan (with the average molecular weight of 500 kD) and 250g of deionized water, and stirring at 10000rpm and 60 ℃ for 5 hours to obtain a spinning solution;
(2) Performing electrostatic spinning on the spinning solution obtained in the step (1), and performing spinning on a silk spunlace non-woven fabric (the thickness of the spunlace non-woven fabric is 0.12 mm) through a spinning nozzle to form a film, so as to obtain the electrostatic spinning mask; the specific parameters of the electrostatic spinning are as follows: the voltage is 10kV, the receiving distance is 10cm, the spinning speed is 0.1mL/h, and the diameter of a needle used for electrostatic spinning is 1.0mm.
Wherein, the hydrolyzed silk is not added in the comparative example 2, so that the hydrolyzed silk is necessarily sprayed on the non-woven fabric substrate; the molecular weight of the schizophyllan must be increased to form the shape without adding the hydrolyzed silk, but the higher feeding amount of the molecular weight causes more solvents and higher shearing speed to ensure that a uniform solution can be formed, otherwise, a spinning nozzle is easily blocked during electrostatic spinning; in addition, the electrospinning parameters are also adjusted adaptively.
Comparative example 3
The comparative example provides an electrostatic spinning mask, which is prepared by the following method:
(1) Mixing 7g of hyaluronic acid (average molecular weight is 300 kD) and 75g of deionized water, stirring at the rotating speed of 4000rpm for 1.5h at 80 ℃, adding 18g of hydrolyzed silk, and stirring at the rotating speed of 2000rpm for 1h at 60 ℃ to obtain a spinning solution;
(2) Performing electrostatic spinning on the spinning solution obtained in the step (1), and performing spinning on a silk spunlace non-woven fabric (the thickness of the spunlace non-woven fabric is 0.12 mm) through a spinning nozzle to form a film, so as to obtain the electrostatic spinning mask; the specific parameters of the electrostatic spinning are as follows: the voltage is 15kV, the receiving distance is 15cm, the spinning speed is 0.5mL/h, and the diameter of a needle used for electrostatic spinning is 0.6mm.
Among them, comparative example 3, in which schizophyllan was not added, was replaced with hyaluronic acid, so that it was necessary to spray it on a nonwoven fabric substrate.
Comparative example 4
The comparative example provides an electrostatic spinning mask, which is prepared by the following method:
(1) Mixing 7g of schizophyllan (with the average molecular weight of 300 kD) and 75g of deionized water, stirring at the rotating speed of 4000rpm for 1.5h at 80 ℃, adding 18g of hydrolyzed collagen, and stirring at the rotating speed of 2000rpm for 1h at 60 ℃ to obtain a spinning solution;
(2) Carrying out electrostatic spinning on the spinning solution obtained in the step (1) to obtain a fiber membrane;
the specific parameters of the electrostatic spinning are as follows: the voltage is 15kV, the receiving distance is 15cm, the spinning speed is 0.2mL/h, and the diameter of a needle used for electrostatic spinning is 0.6mm; and finally, placing the fiber membrane formed by electrostatic spinning in a low-voltage electrostatic field with the field strength of 500V/m, and performing sub-supercooling treatment at the temperature of minus 20 ℃ to obtain the electrostatic spinning facial mask.
Test example 1
Irritation testing machine evaluation method (skin seal patch test)
Test samples: spinning solutions provided in examples 1-8 and comparative examples 1-4;
the test method comprises the following steps: 1. the subjects were enrolled with 120 panelists selected for inclusion criteria and randomized into 12 groups of 10 panelists each. 2. A qualified spot tester was selected, the spinning solutions provided in examples 1 to 8 and comparative examples 1 to 4 were diluted to 10mg/mL with 20mmoL/L PBS solution, respectively, and used as sample solutions, 0.05mL of the spinning solutions were dropped into the spot tester, and one group of the spinning solutions was selected as a blank control (0 mmoL/L PBS solution was used as a blank control), and the spot tester was taped to the forearm of the subject for 24 hours. 3. Respectively observing skin reactions 48 hours after the test object spot tester is removed, wherein the skin reaction grading standard of the skin closed type spot test is shown in table 1, and the specific test result is shown in table 2:
TABLE 1
Figure BDA0003435408280000101
Figure BDA0003435408280000111
TABLE 2
Figure BDA0003435408280000112
As can be seen from the test results in Table 1, in the skin sealing patch test, after the spinning solutions provided in examples 1 to 8 of the present invention and comparative examples 1 to 4 were applied for 48 hours, the subjects did not show any reaction and no adverse reaction, such as erythema, burning sensation or itching. The enclosed patch test shows that the mask matrix has no irritation to skin.
Test example 2
Skin moisture content testing
Test samples: the electrospun masks provided in examples 1-8 and comparative examples 1-4;
the test principle is as follows: the probe of the skin moisture content tester is used for testing based on the principle of capacitance, and the moisture content testing probe is used for measuring the capacitance value of the skin and analyzing the moisture content of the surface of the skin;
testing population: 200 dry skin people (people with the accumulated stinging sensation more than or equal to 3 points) are selected, the age is 18-50 years old, and the age is half of that of men and women. The groups were randomized into 10 groups of 10 males and 10 females. And the test period (within 15 days) is not coated with any drug or cosmetic which is irrelevant to the experiment. The test environment temperature is controlled to be 25 +/-1 ℃, and the relative humidity is 40 +/-5%;
the test method comprises the following steps: before the test, detecting the skin moisture content of the testee as a basic value, after each group of testee cleans the face, respectively using the facial masks of the corresponding group on the face, continuously using for 4h and 8h, and testing the skin moisture loss degree by using a skin moisture loss tester (Biox Aquaflus), wherein the data is an average value of all data in the same test group;
the specific test results are shown in table 3:
TABLE 3
Figure BDA0003435408280000121
Figure BDA0003435408280000131
From the test results in table 3, the skin moisture content of the subjects was increased after using the electrostatic spinning mask of the present invention, and compared with the basic value (0 h, before use), the skin moisture content was increased by at least 40% after 4h, and as a preferred technical solution (examples 1-3), the skin moisture content was increased to more than 52%, indicating that the electrostatic spinning mask of the present invention has high moisturizing effect. The moisturizing ability of the electrospun masks provided in comparative examples 1-4 was not ideal. The electrostatic spinning mask can well exert the effects of all components in the hydrogel matrix, and achieves full-effect moisture preservation and care of reducing the transdermal water loss rate, enhancing the internal cell water circulation, strengthening the surface water-locking barrier and the like.
Test example 3
Skin brightness test
Test samples: the electrospun masks provided in examples 1-8 and comparative examples 1-4;
testing the population: 200 volunteers were selected, aged 18-50 years. Groups were randomized into 10 groups of 20 women. And the test period (within 15 days) does not apply any drug or cosmetic which is irrelevant to the experiment. The test environment temperature is controlled to be 25 +/-1 ℃, and the relative humidity is 40 +/-5%;
the test method comprises the following steps: before the test, the skin water content of the test subjects is detected as a basic value, after each group of test subjects clean the face at night, the corresponding group of facial masks are respectively used on the face, and after the test subjects continuously use for 2 weeks and 4 weeks, the skin brightness (L value) is measured by a skin water loss tester (Biox Aquaflus) and a facial skin image analyzer (VISIA-CR);
the specific test results are shown in table 4:
TABLE 4
Figure BDA0003435408280000141
As can be seen from the test results in table 4, the skin brightness (L value) of the subjects was increased after using the electrostatic spinning mask of the present invention, and the skin moisture content was increased by at least 2% after four weeks as compared with the base value (week 0), and was increased to 3% or more as a preferred embodiment (examples 1 to 3), indicating that the electrostatic spinning mask of the present invention has an efficient whitening effect. And the whitening ability of the electrospun masks provided in comparative examples 1 to 4 is not ideal.
Test example 4
Skin elasticity test
Test samples: the electrospun masks provided in examples 1-8 and comparative examples 1-4;
the test principle is as follows: the skin elasticity tester MPA580 from CK, germany was used to suck the skin into a specific test probe by measuring the negative pressure generated on the skin surface before and after use of the product, the depth to which the skin was sucked into the test probe being measured by a non-contact optical test system. The test probe comprised a transmitter and receiver of light, the ratio of which was proportional to the depth of the skin being inhaled, and then analyzed by the MPA software to determine the elastic properties of the skin. The ratio of the resilience of the skin without negative pressure to the maximum stretching amount with negative pressure is closer to 1, which indicates that the skin has better elasticity;
the test method comprises the following steps: 200 dry skin people (people with the accumulated stinging sensation more than or equal to 3 points) are selected, the age is 18-50 years old, and the age is half of that of men and women. The groups were randomized into 10 groups of 10 males and 10 females. The test method comprises the following steps: in the test, a half-face test is carried out, and the same volunteer and use method are carried out in the period of 0 week, 2 weeks and 4 weeks for return visit, and VISIA image shooting and elasticity test are carried out after the patient sits statically in a constant temperature and humidity environment for 30 min. And then the average elasticity data of the volunteers at different time intervals are obtained through calculation.
The specific test results are shown in table 5:
TABLE 5
Figure BDA0003435408280000151
Figure BDA0003435408280000161
From the test results in table 5, it can be seen that the skin elasticity of the subjects is increased after the mask of the present invention is applied, and the skin moisture content is increased by at least 69% or more after four weeks compared with the base value (week 0), and can be increased to 90% or more as a preferred embodiment (examples 1 to 3), indicating that the mask of the present invention has the capability of improving the skin elasticity. While the electrospinning masks provided in comparative examples 1-4 had unsatisfactory skin elasticity-improving ability. The mask disclosed by the invention can be used for improving skin nutrition metabolism, maintaining skin elasticity and simultaneously repairing epidermal tissues, so that multiple effects of moisturizing, wrinkle resistance and aging resistance are achieved.
Test example 5
Skin wrinkle resistance test
Test samples: the electrospun masks provided in examples 1-8 and comparative examples 1-4;
testing the population: 200 volunteers were selected, aged 18-50 years. Groups were randomized into 10 groups of 20 women. And the test period (within 15 days) is not coated with any drug or cosmetic which is irrelevant to the experiment. The test environment temperature is controlled to be 25 +/-1 ℃, and the relative humidity is 40 +/-5%;
the test method comprises the following steps: before the test, detecting the skin moisture content of the test subjects as a basic value, after each group of test subjects clean the face at night, respectively using the facial masks of the corresponding group on the face, continuously using for 1 month and 3 months, testing the face wrinkle condition by using a face skin image analyzer (VISIA-CR), and analyzing the wrinkle reduction amount;
the specific test results are shown in table 6:
TABLE 6
Figure BDA0003435408280000171
The test results in table 6 show that the electrostatic spinning mask has a good anti-wrinkle function, the average wrinkle amount of the face after 1 month of use is reduced by more than 16%, the average eye line amount after 3 months of use is reduced by more than 30%, the average eye line volume after 1 month of use is reduced by more than 15%, and the average eye line amount after 3 months of use is reduced by more than 30%. And the anti-wrinkle effect of the electrostatic spinning mask provided by the comparative examples 1 to 4 is not ideal. The mask provided by the invention can improve skin nutrition metabolism, keep skin elasticity and repair epidermal tissues, so that multiple effects of moisturizing, wrinkle resistance and aging resistance are achieved.
The applicant states that the present invention is illustrated by the above examples to describe the electrospun mask of the present invention and the preparation method thereof, but the present invention is not limited to the above examples, i.e., it does not mean that the present invention must be implemented by the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims (9)

1. The electrostatic spinning facial mask is characterized by comprising an electrostatic spinning fiber membrane formed by schizophyllan and hydrolyzed silk;
the mass ratio of the schizophyllum commune polysaccharide to the hydrolyzed silk is (0.1-10) to (5-30); the molecular weight of the schizophyllan is 100-1000 kD.
2. The electrospun mask of claim 1 wherein the mass ratio of the schizophyllan to the hydrolyzed silk is (5-10) to (15-20).
3. The electrospun mask of claim 1 wherein the molecular weight of the schizophyllan is 200-400kD.
4. The electrostatic spinning mask pack as claimed in claim 1, wherein the raw materials for preparing the electrostatic spinning fiber film comprise the following components in percentage by mass: 0.1-10% of schizophyllan, 5-30% of hydrolyzed silk and the balance of water.
5. The method for preparing an electrospun facial mask according to any one of claims 1 to 4, comprising the steps of:
(1) Mixing the schizophyllum commune polysaccharide, the hydrolyzed silk and water, and stirring to obtain a spinning solution;
(2) Injecting the spinning solution obtained in the step (1) in an electric field, wherein the specific parameters of electrostatic spinning are as follows: the voltage is 15-25kV, the receiving distance is 10-20cm, the spinning speed is 0.1-1mL/h, and after electrostatic spinning, the electrostatic spinning mask is obtained by collecting through a collecting device.
6. The method for preparing an electrospun mask pack according to claim 5, wherein in the step (1), the rotation speed of the agitation is 1000-5000 rpm.
7. The method for preparing an electrospun facial mask according to claim 5, wherein in the step (1), the stirring temperature is 40-90 ℃ and the stirring time is 0.5-5 h.
8. The method for preparing an electrospinning mask pack according to claim 5, wherein in the step (1), the specific preparation method of the spinning solution is as follows: firstly mixing schizophyllan and water, stirring for 0.5-2h at the rotating speed of 3000-5000rpm and the temperature of 50-90 ℃, adding hydrolyzed silk, and stirring for 0.5-3h at the rotating speed of 1000-3000rpm and the temperature of 40-60 ℃ to obtain a spinning solution.
9. The method of preparing an electrospinning mask pack according to claim 5, wherein in the step (2), the electrospinning needle has a diameter of 0.5 to 1 mm.
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