CN112915034A - Silk fibroin nanofiber instant mask and preparation method thereof - Google Patents
Silk fibroin nanofiber instant mask and preparation method thereof Download PDFInfo
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
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- A61K8/345—Alcohols containing more than one hydroxy group
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
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- D01D5/0084—Coating by electro-spinning, i.e. the electro-spun fibres are not removed from the collecting device but remain integral with it, e.g. coating of prostheses
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
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Abstract
The invention discloses a silk fibroin nanofiber instant mask and a preparation method thereof, the 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 the following components in parts by weight: 1-30 parts of silk fibroin, 0.1-3 parts of lower polyhydric alcohol and 0.1-5 parts of surface active substances; the mask electrostatic spinning matrix takes purified water as a solvent, and is environment-friendly and safe. Diffusion and permeation experiments show that after the mask disclosed by the invention is used, the absorption effect of skin on collagen macromolecules is obvious.
Description
Technical Field
The invention relates to a facial mask and a preparation method thereof, in particular to an instant facial mask containing silk fibroin nanofibers and a preparation method thereof.
Background
In the cosmetic market, mask products for personal care are mostly in the form of supporting essence on non-woven fabrics, but such products also have various disadvantages when used. People are constantly developing new facial masks to meet the ever-changing consumer demands of the market.
For example, chinese patent 201310366143.X discloses a composite nanofiber membrane, a preparation method and applications thereof, which includes the steps of: (1) dissolving any one of polyvinyl alcohol, polylactic acid and regenerated silk fibroin in an organic solvent to prepare spinning solution with the mass fraction of 5-20%; (2) adding a polyphenol substance into the spinning solution, and uniformly stirring to obtain a mixed spinning solution which accounts for 1-7% of the total mass of the polyphenol substance and the organic solvent, wherein the polyphenol substance is one or more of plant tannin, apple polyphenol and grape polyphenol; (3) carrying out ultrasonic treatment on the mixed spinning solution for 1-600 min; (4) and (3) carrying out electrostatic spinning on the mixed spinning solution, and collecting to obtain the required composite nanofiber membrane. However, the spinning solution of the patent is prepared by an organic solvent, which brings more environmental protection problems.
Chinese patent application 201910371938.7 discloses a novel sheet-like facial mask, its preparation method and application method, wherein the sheet-like facial mask comprises hydrophilic nanofiber layer and hydrophobic nonwoven fabric layer. The hydrophilic nanofiber layer is prepared by an electrospinning method and comprises the following steps: (1) dissolving a hydrophilic polymer in an organic solvent, and stirring at room temperature to obtain a solution A; wherein, the hydrophilic polymer can be polyvinyl alcohol, polyethylene glycol, polymethacrylamide and regenerated silk fibroin, and the mass percentage concentration is 10-20%; (2) and (3) stirring at room temperature, and directly performing electrostatic spinning on the hydrophobic non-woven fabric to obtain the nanofiber mask with the double-layer structure. Likewise, water is the most environmentally friendly and cost effective solvent compared to organic or other non-polar solvents, but organic solvents are preferred.
In the prior art, when the nanofiber is prepared by utilizing electrostatic spinning, on one hand, the formed nanofiber is easy to have the phenomena of agglomeration, knots, broken filaments, cavities and the like, the structure of the nanofiber is seriously influenced, and the care performance of a mask is reduced, on the other hand, the nutrient components added in the spinning solution often influence the formation of the spinning fiber, and the solvent selection of the spinning solution also often neglects the problem of environmental protection.
Chinese patent application 201910052945.0 discloses a collagen nano instant facial mask using hyaluronic acid as a skeleton and a preparation method thereof, wherein a nanofiber layer is formed on a non-woven fabric substrate layer by an electrostatic spinning method, and the nanofiber layer comprises sodium hyaluronate, hydrolyzed collagen and a surface active substance; wherein the average molecular weight of the sodium hyaluronate is 20000-60000, and the average molecular weight of the hydrolyzed collagen is 1000-3000. The patent application technology can overcome the defects of the prior art and has excellent care performance of the mask.
Chinese patent application 201910053466.0 discloses a collagen nano instant facial mask using pullulanase as a skeleton and a preparation method thereof, wherein a nanofiber layer is formed on a non-woven fabric substrate layer by adopting an electrostatic spinning method, and the nanofiber layer comprises: 10-60 parts of pullulanase polysaccharide and 5-40 parts of hydrolyzed collagen with lower molecular weight; and 0.1 to 5 parts by weight of a surface active substance; wherein the average molecular weight of the pullulanase polysaccharide is between 100000-300000, and the average molecular weight of the hydrolyzed collagen with lower molecular weight is between 1000-3000.
In order to make the nursing components in the facial mask product have better biocompatibility with human body, the application of silk fibroin in the field of cosmetics has gained attention in recent years. It is found that silk fibroin is greatly different from common animal collagen: from the structure, the silk fibroin belongs to macromolecular collagen peptide, the molecular weight can be customized according to the requirement, and the animal collagen (gelatin) is a micromolecular hydrolysate; from the production process, the silk fibroin can be extracted and purified in aqueous solution, and the animal collagen is mainly prepared by an enzymolysis method, so that the steps are complicated, and the quality control is difficult; from the aspect of biological activity, the special spatial structure of silk fibroin leads the silk fibroin to have biological activity, and most animal glue has no activity or very low activity; from the aspect of affinity with human, silk fibroin has good affinity, but the affinity of animal collagen is poor; from the aspect of skin barrier effect, silk fibroin has the skin barrier effect, and animal collagen does not have the skin barrier effect; from the aspect of promoting cell growth, silk fibroin can promote cell growth rapidly, and the cell growth of animal collagen is slow or none; from the aspect of the skin wrinkle-removing effect, silk fibroin has a strong skin wrinkle-removing effect, and the skin wrinkle-removing effect of animal collagen is weak; from the perspective of antianaphylaxis, silk fibroin can form a film to isolate an allergen and can help repair the dermal layer structure of the skin, and animal glue has no effect or even has slight sensitization; from the hidden biological safety, silk fibroin has no biological safety hidden trouble, and the animal glue principle may have virus; from the point of immunogenicity (rejection), silk fibroin has no rejection, while zooglea may have rejection in principle.
For example, chinese patent application CN201810551731.3 discloses a silk-like gel mask and a preparation method thereof, wherein the mask comprises a base fabric layer and a substrate layer, the base fabric layer is a copper ammonia fiber layer, and the substrate layer is a silk-like gel layer. The invention utilizes a centrifugal spinning method, when a spinning nozzle reaches a certain rotating speed, silk fibroin-hyaluronic acid spinning solution containing a cross-linking agent, an antibacterial component and an antioxidant component is thrown out of the spinning nozzle, is rapidly cross-linked at the temperature of 25-60 ℃ to form filamentous gel filaments with the diameter of 1-5um, and is deposited on the surface of the copper ammonia fiber base cloth layer under the action of gravity. However, the invention adopts a centrifugal spinning method, the obtained gel filament is not nanofiber, and the exertion of the nursing efficacy of the silk fibroin is greatly influenced.
For another example, chinese patent application CN201611126194.5 discloses a hyaluronic acid/silk fibroin nanofiber and a method for preparing the same, wherein hyaluronic acid and silk fibroin are made into an electrostatic spinning mixed solution, and essential oil and vitamin C are added for blending, so as to obtain the hyaluronic acid/silk fibroin nanofiber capable of slowly releasing essential oil and vitamin C. However, in the invention, the silk fibroin is dissolved in a mixed solvent of glacial acetic acid and N, N-dimethylacetamide in a volume ratio of 1:2 to prepare the silk fibroin spinning solution, i.e., the invention still utilizes an organic solvent, otherwise, high-quality silk fibroin nanofibers cannot be obtained.
Therefore, there is a need to provide a facial mask with good biocompatibility of main care components and human body and environmentally friendly preparation process, so as to overcome the disadvantages and shortcomings of the prior art.
Disclosure of Invention
The invention aims to provide a dry facial mask with silk fibroin as a main nursing component and a preparation method thereof.
In one aspect, in order to achieve the above object, the present invention provides a collagen nano instant facial mask containing silk fibroin, the facial mask including a non-woven fabric substrate layer and a nanofiber layer, wherein the nanofiber layer is formed on the non-woven fabric substrate layer by an electrostatic spinning method, and the nanofiber layer includes:
1-30 parts of silk fibroin, preferably 1-20 parts of silk fibroin;
0.1 to 3 parts by weight of a lower polyol, preferably 0.2 to 1 part by weight of a lower polyol; and
0.1 to 5 parts by weight of a surface-active substance, preferably 0.1 to 2 parts by weight of a surface-active substance;
wherein, the solvent adopted by the spinning solution of electrostatic spinning is pure water; the average molecular weight of the silk fibroin is 20000-80000, preferably 30000-50000; the surface-active substances used are water-soluble, skin-caring and electrospun.
In the silk fibroin nanofiber facial mask, silk fibroin used by the facial mask is a main component of silkworm silk, a single silk is formed by bonding two parallel silk fibroin monofilament fibers, and sericin is used as a substance in the middle and the periphery of the fibers for bonding and wrapping. The silk fibroin accounts for 70-80% of the silk, and the sericin accounts for 20-30%. The silk fibroin obtained by removing sericin from silk contains 18 kinds of amino acids including 8 kinds necessary for human body, wherein the amino acids with moisture keeping and radiation preventing functions such as glycine, alanine, serine, tyrosine, etc. account for more than 80% of the total amount of the 18 kinds of amino acids.
The silk fibroin adopted by the invention has good biocompatibility, does not have inflammation and immunoreaction when being injected or transplanted into an animal body in the medical field, and has more excellent biological safety and mechanical, degradation, drug slow release and other performances compared with the traditional biological material products such as collagen, hyaluronic acid and the like, thereby being widely applied to the research and development of medical instruments and drug slow release products. Compared with the medical field, the silk fibroin is easier to be widely popularized and applied in the fields of skin care products and health care products due to the excellent material performance and abundant material sources. Silk fibroin has been included in food and cosmetic catalogues under the names of fibroin, silk powder, silk peptide, silk extract, etc., and thus, unlike medical products, skin care products and health care products made with silk fibroin present no regulatory barriers.
In the silk fibroin nanofiber mask, silk fibroin can form a framework, or form the framework together with other substances, or form the framework by other substances, and the purposes and the technical effects of the silk fibroin nanofiber mask can be realized. The silk fibroin can form the skeleton of the nano fiber and can also be used as the skin care active ingredient.
The present inventors have surprisingly found that when electrospinning using an aqueous solution of silk fibroin as a spinning solution, it is difficult to smoothly produce non-aggregated, uniform silk fibroin nanofibers without adding appropriate amounts of a lower polyol and a surface active substance, particularly a lower polyol, if the lower polyol (e.g., C) is contained in the raw material for forming the silk fibroin nanofibers2-C6Polyol) and surface active substances, the smooth proceeding of electrostatic spinning can be ensured, the agglomeration in the spinning process is prevented, and the uniformity of the obtained silk fibroin nano-fiber is ensured。
In the silk fibroin nanofiber mask pack of the present invention, the small amount of lower polyol used is preferably C2-C6Such as ethylene glycol, propylene glycol, butylene glycol, etc., and the presence of such a lower polyol not only facilitates the spinning process but also has certain skin care functions such as moisturizing effect, etc. by itself.
In the silk fibroin nanofiber mask of the present invention, the main role of the surfactant used is to reduce surface tension, but not any surfactant is suitable for the present invention; the surface-active substances according to the invention should be water-soluble, have no adverse effect on the skin care and should not interfere with the electrospinning to form uniform fibers. That is, in the present invention, any surface active material that is water-soluble, has a certain skin care effect, and facilitates electrospinning can be used in the present invention.
As a specific embodiment of the present invention, in the silk fibroin nanofiber facial mask of the present invention, the nanofiber layer may further include:
0.1-10 parts by weight of sodium hyaluronate;
wherein the average molecular weight of the sodium hyaluronate is 20000-60000, preferably 25000-50000; the weight ratio of the silk fibroin to the sodium hyaluronate can be controlled to be 100: 1 to 1: 100, preferably controlled between 100: 1 to 10: 100, more preferably between 100: 10 to 10: 100, respectively.
As another embodiment of the present invention, in the silk fibroin nanofiber facial mask of the present invention, the nanofiber layer may further include:
1-25 parts by weight of pullulanase;
wherein the average molecular weight of the pullulanase polysaccharide used is between 100000-300000, preferably between 150000-250000, such as between 170000-230000; the weight ratio of silk fibroin to pullulanase can be controlled to be 80: 1 to 1: 80, preferably controlled between 80: 3 to 3: 80, more preferably between 80: 10 to 10: 80.
As still another embodiment of the present invention, in the silk fibroin nanofiber facial mask of the present invention, the nanofiber layer may include:
1-20 parts by weight of silk fibroin;
0.1-10 parts by weight of sodium hyaluronate;
1-20 parts by weight of pullulanase;
0.2-1 parts by weight of a lower polyhydric alcohol; and
0.1-2 parts by weight of a surface active substance;
wherein, the silk fibroin: the weight ratio of (sodium hyaluronate + pullulanase) can be controlled to be 60: 1 to 1: 60, preferably between 60: 3 to 3: 60 is between; and sodium hyaluronate: the weight ratio of the pullulanase polysaccharide can be controlled to be 20: 1 to 1: 20, respectively.
The electrostatic spinning technology adopted by the invention is a construction technology that a polymer solution overcomes surface tension under the action of high-voltage static electricity, forms a Taylor (Taylor) cone at a spinning nozzle, jets out jet flow at high speed, and is solidified to form a nanofiber structure through mechanical stretching and solvent volatilization.
The nanofiber layer in the facial mask can be a layered object which is prepared by taking water-soluble polymers such as silk fibroin, sodium hyaluronate, pullulanase and the like as substrates through an electrostatic spinning technology and is formed by fibers with diameters of only hundreds of nanometers, and the facial mask has the advantages of large specific surface area, good fiber continuity, small fiber membrane aperture, high porosity and the like, has good effects of slow release and protection of active substances, is easy to permeate skin cuticle to reach the deep layer of the skin, and has the functions of moisturizing, whitening, aging delaying and the like.
In order to form uniform spinning and prevent the occurrence of a lumping phenomenon during the electrospinning process, it is preferable that the nanofiber layer thereof further comprises, in the mask pack of the present invention: 0.05-5 parts by weight of maltooligosaccharide glucoside and 0.03-3 parts by weight of hydrogenated starch hydrolysate, preferably 0.5-5 parts by weight of maltooligosaccharide glucoside and 0.3-3 parts by weight of hydrogenated starch hydrolysate. The use of maltooligosaccharide glucoside and hydrogenated starch hydrolysate improves the user's use of the mask of the present invention, which prevents the occurrence of a slushing phenomenon on the face. In the nanofiber layer of the mask of the present invention, if the ratio of maltooligosaccharide glucoside to hydrogenated starch hydrolysate used is too low, the above-mentioned improvement effect is not significant, but if the ratio is too high, the spinning performance is adversely affected, for example, the fiber strength is too low, the skin care effect is reduced, and the like.
Preferably, in the mask pack of the present invention, the nanofiber layer further comprises: 0.1 to 4 parts by weight of polyethylene glycol having a high degree of polymerization, and 0.1 to 2 parts by weight of polyethylene glycol having a low degree of polymerization, preferably 0.1 to 2 parts by weight of polyethylene glycol having a high degree of polymerization, and 0.2 to 2 parts by weight of polyethylene glycol having a low degree of polymerization; wherein the average molecular weight of the polyethylene glycol with high polymerization degree is 250000-350000, and the average molecular weight of the polyethylene glycol with low polymerization degree is 6000-10000.
The polyethylene glycol with high polymerization degree can increase the tenacity of the fiber, so that the spinning becomes relatively easy and the spinning is uniform; the polyethylene glycol with low polymerization degree can further prevent the agglomeration phenomenon in the electrostatic spinning process and promote the formation of uniform spinning.
Preferably, in the mask pack of the present invention, the low-polymerization-degree polyethylene glycol used has an average molecular weight of between 7000 and 9000; more preferably, the polyethylene glycol of low degree of polymerization used has an average molecular weight of between 7600 and 8600.
In the silk fibroin nanofiber facial mask of the present invention, the surface active substances used may be, but are not limited to: polyoxyethylene sorbitol ester type emulsifiers such as polysorbate-20, polysorbate-60, polysorbate-80 and the like; sucrose ester emulsifiers such as sucrose laurate, sucrose stearate; polyglycerin-based emulsifiers such as polyglycerin-10 myristate, polyglycerin-6 caprylate, polyglycerin-6 stearate, and the like; glycoside emulsifiers such as coco glucoside, lauryl glucoside, and the like; polyether or polyether ester emulsifiers such as PEG-40 hydrogenated castor oil, PEG-20 methylgluco-sesquistearate, etc.; and so on.
As a specific embodiment of the present invention, in the silk fibroin nanofiber facial mask of the present invention, the nanofiber layer thereof comprises:
5-25 parts by weight of silk fibroin;
1-10 parts by weight of sodium hyaluronate;
0.5-5 parts by weight of maltooligosaccharide glucoside;
0.3-3 parts by weight of a hydrogenated starch hydrolysate;
0.1-2 parts by weight of polyethylene glycol having a high degree of polymerization;
0.2 to 2 parts by weight of polyethylene glycol having a low degree of polymerization;
0.2-1 parts by weight of a lower polyhydric alcohol; and
0.1-2 parts by weight of a surface-active substance.
As another specific embodiment of the present invention, in the silk fibroin nanofiber facial mask of the present invention, the nanofiber layer thereof comprises:
5-25 parts by weight of silk fibroin;
2-20 parts by weight of pullulanase;
0.5-5 parts by weight of maltooligosaccharide glucoside;
0.3-3 parts by weight of a hydrogenated starch hydrolysate;
0.1-2 parts by weight of polyethylene glycol having a high degree of polymerization;
0.2 to 2 parts by weight of polyethylene glycol having a low degree of polymerization;
0.1 to 3 parts by weight of a lower polyhydric alcohol; and
0.1-2 parts by weight of a surface-active substance.
In addition, to further increase the skin care activity of the nanofiber layer, part of the silk fibroin may be replaced with yeast recombinant collagen. For example, the nanofiber layer of the mask of the present invention comprises:
1-30 parts by weight of silk fibroin;
0.1-10 parts by weight of yeast recombinant collagen;
0.1 to 3 parts by weight of a lower polyhydric alcohol; and
0.1 to 5 parts by weight of a surface-active substance;
wherein the average molecular weight of the yeast recombinant collagen is 20000-100000, preferably 40000-80000. Or the nanofiber layer of the mask of the present invention comprises:
1-20 parts by weight of silk fibroin;
1-5 parts by weight of yeast recombinant collagen;
0.1 to 3 parts by weight of a lower polyhydric alcohol; and
0.1 to 5 parts by weight of a surface-active substance;
in the mask pack of the present invention, a peelable protective layer may be further included on the nanofiber layer. In this product design, the final product has three layers, a nonwoven fabric as the backing, electrospun onto the nonwoven fabric backing, the filaments formed by electrospinning being the middle layer (nanofiber layer) and the outer layer having a coating, which may be a PE film or a BOPP film, but which requires static removal. When the product is used, the fiber layer is not required to be stripped, and the product can be used only by uncovering the coating film on the outer surface; the product can be mixed with nutrient solution or not, and consumers can use the product only by spraying pure water on the face.
Further, in the mask pack of the present invention, the nanofiber layer may include 0.001-2 parts by weight of a functional substance, such as a preservative, e.g., pentasodium penta-pentetate, phytic acid, silver oxide, etc., or other skin care agents, etc.
In another aspect, to achieve the object of the present invention, the present invention also provides a method for preparing the above mask, wherein the method comprises the steps of:
(1) and preparing a spinning solution: adding silk fibroin and surface active substances into purified water as a solvent, and stirring to form uniform spinning solution, wherein the spinning solution comprises 1-30 wt% of silk fibroin, 0.1-3 wt% of lower polyhydric alcohol and 0.1-5 wt% of surface active substances;
(2) and electrostatic spinning: adding the prepared spinning solution into electrostatic spinning equipment, and carrying out electrostatic spinning by taking non-woven fabrics as a receiving base material;
wherein the average molecular weight of the silk fibroin is 20000-80000, preferablyBetween 30000 and 50000; the lower polyol used is C2-C6The polyol of (1); the surface active substance is water-soluble, has skin care effect, and is beneficial to electrostatic spinning.
In the above method, the spinning solution may further comprise 0.1-10 wt% of sodium hyaluronate or 1-25 wt% of pullulanase polysaccharide, wherein the average molecular weight of the sodium hyaluronate is 20000-60000 and the average molecular weight of the pullulanase polysaccharide is 100000-300000.
Preferably, the spinning solution further comprises: 0.05-5 wt% maltooligosaccharide glucoside, 0.03-3 wt% hydrogenated starch hydrolysate; more preferably, the spinning solution further comprises 0.1-4 wt% of polyethylene glycol with high polymerization degree and 0.1-2 wt% of polyethylene glycol with low polymerization degree, wherein the average molecular weight of the polyethylene glycol with high polymerization degree is 250000-350000, and the average molecular weight of the polyethylene glycol with low polymerization degree is 6000-10000.
The electrostatic spinning equipment used in the preparation process can adopt roller-type needle-free electrostatic spinning equipment, and the equipment has the characteristics of large spinning quantity, high production efficiency and uniform spinning.
The facial mask is a dry facial mask, and the efficacy test method comprises the following steps of comparing a silk fibroin collagen nano instant facial mask solution with a silk fibroin collagen nano instant dry facial mask by utilizing the back skin of a suckling pig based on a Franz diffusion cell, and evaluating the efficacy difference of the silk fibroin collagen nano instant dry facial mask in the aspects of promoting collagen permeation and skin absorption by evaluating the permeation behavior of collagen components in vitro skin. The result shows that the mask of the invention has the advantages that the sample is mostly concentrated at the stratum corneum part at the beginning of 2h, the sample gradually enters the living cell layer from the stratum corneum after 4h-6h, and the sample can be seen to enter the dermis after 24 h. In addition, in the whole process, the collagen signal detectable by the silk fibroin collagen nano instant dry facial mask group at the same time point is higher than that of the silk fibroin collagen nano instant facial mask solution, especially in 24 hours. This shows that the silk fibroin collagen nano instant dry facial mask of the invention promotes the absorption of collagen macromolecules by skin.
The present invention will be further described with reference to the accompanying drawings and specific embodiments, which are illustrative of certain specific embodiments of the present invention and are not to be construed as limiting the invention.
Drawings
FIG. 1 is a schematic diagram of Franz diffusion cell operation;
FIG. 2 shows the trend of the results of the fluorescence data analysis of the diffusion permeation assay (by sample);
FIG. 3 shows the trend of the results of the fluorescence data analysis (in time) of the diffusion permeation experiment;
detailed description of the preferred embodiments
Example 1
The mask of the present invention is prepared as follows:
(1) preparing a spinning solution: adding silk fibroin (from Simeite biotechnology, Inc. of Suzhou), sodium hyaluronate, maltooligosaccharide glucoside, hydrogenated starch hydrolysate, PEG-7M, PEG-180, polyglycerol-10 myristate, pullulanase and preservative into pure water serving as a solvent, and stirring in a constant-temperature water bath at 20-50 ℃ for 2-6 hours until the solution is uniform and free of particles to obtain a spinning solution containing the following components: 18 wt% of silk fibroin, 0.2 wt% of sodium hyaluronate, 2.0 wt% of pullulanase polysaccharide, 2.4 wt% of maltooligosaccharide glucoside, 1.4 wt% of hydrogenated starch hydrolysate, 0.5 wt% of PEG-7M, 0.3 wt% of PEG-180, 0.2 wt% of glycerol, 0.1 wt% of polyglycerol-10 myristate, and 1.0 wt% of preservative, wherein the average molecular weight of the sodium hyaluronate used is about 30000, the average molecular weight of the silk fibroin used is about 20-80KDa, the average molecular weight of the PEG-7M used is about 300000, the average molecular weight of the PEG-180 used is about 8000, the molecular weight of the pullulanase polysaccharide used is 200000, and the preservative used is pentetate, inositol hexaphosphate, silver oxide;
(2) and electrostatic spinning: pouring the prepared uniform solution into a trough of electrostatic spinning equipment, controlling the humidity of a spinning environment to be 30-50%, the spinning distance to be 140-220 mm, the spinning voltage to be 40-85 KV, the spinning speed to be 0.1-1.2 r/min and the current to be 0.2-1.5mA, and carrying out electrostatic spinning by taking non-woven fabrics as a receiving base material.
Example 2
A mask was prepared in the same procedure and manner as in example 1, except that the prepared dope contained the following components: 10 wt% of silk fibroin, 3 wt% of sodium hyaluronate, 1.0 wt% of pullulanase polysaccharide, 0.5 wt% of maltooligosaccharide glucoside, 0.5 wt% of hydrogenated starch hydrolysate, 0.5 wt% of PEG with high polymerization degree, 5 wt% of PEG with low polymerization degree, 3 wt% of butanediol, 5.0 wt% of polysorbate-20 and 0.1 wt% of preservative, wherein the average molecular weight of the silk fibroin used is about 40-80KDa, the average molecular weight of the sodium hyaluronate used is about 25000, the molecular weight of the pullulanase polysaccharide used is 250000, the average molecular weight of the PEG with high polymerization degree is about 250000, and the average molecular weight of the PEG with low polymerization degree is about 10000.
Example 3
A mask was prepared in the same procedure and manner as in example 1, except that the prepared dope contained the following components: 5 wt% of silk fibroin, 5 wt% of sodium hyaluronate, 5.0 wt% of pullulanase polysaccharide, 3 wt% of maltooligosaccharide glucoside, 1.7 wt% of hydrogenated starch hydrolysate, 1 wt% of PEG with high polymerization degree, 2 wt% of PEG with low polymerization degree, 1.0 wt% of ethylene glycol, 0.2 wt% of sucrose laurate and 2.0 wt% of preservative, wherein the average molecular weight of the silk fibroin used is about 40-80KDa, the average molecular weight of the sodium hyaluronate used is about 50000, the molecular weight of the pullulanase polysaccharide used is 150000, the average molecular weight of the PEG with high polymerization degree used is about 350000, and the average molecular weight of the PEG with low polymerization degree used is about 9000.
Example 4
A mask was prepared in the same procedure and manner as in example 1, except that the prepared dope contained the following components: the silk fibroin-containing coating comprises, by weight, 3% of silk fibroin, 10% of sodium hyaluronate, 5% of maltooligosaccharide glucoside, 3% of hydrogenated starch hydrolysate, 4% of PEG with high polymerization degree, 2% of PEG with low polymerization degree, 0.8% of propylene glycol, 3% of coco glucoside and 1.0% of preservative, wherein the average molecular weight of the silk fibroin is about 40-80KDa, the average molecular weight of the sodium hyaluronate is about 55000-60000, the average molecular weight of the PEG with high polymerization degree is about 280000, and the average molecular weight of the PEG with low polymerization degree is about 7000.
Example 5
A mask was prepared in the same procedure and manner as in example 1, except that the prepared dope contained the following components: 25 wt% of silk fibroin, 1.0 wt% of pullulanase polysaccharide, 2 wt% of maltooligosaccharide glucoside, 1.2 wt% of hydrogenated starch hydrolysate, 0.1 wt% of high-polymerization-degree PEG, 0.1 wt% of low-polymerization-degree PEG, 0.6 wt% of hexanediol, 1.5 wt% of PEG-40 hydrogenated castor oil and 0.5 wt% of preservative, wherein the average molecular weight of the silk fibroin used is about 40-80KDa, the molecular weight of the pullulanase polysaccharide used is 170000, the average molecular weight of the high-polymerization-degree PEG used is 320000, and the average molecular weight of the low-polymerization-degree PEG used is 7600.
Example 6
A mask was prepared in the same procedure and manner as in example 1, except that the prepared dope contained the following components: 10 wt% silk fibroin, 2 wt% sodium hyaluronate, 4 wt% maltooligosaccharide glucoside, 2.5 wt% hydrogenated starch hydrolysate, 0.3 wt% high polymerization degree PEG, 0.3 wt% low polymerization degree PEG, 0.25 wt% butanediol, 1.8 wt% polyglycerol-6 caprylate, and 0.3 wt% preservative, wherein the average molecular weight of the used silk fibroin is about 40-80KDa, the average molecular weight of the used sodium hyaluronate is about 33000, and the used high polymerization degree PEG and low polymerization degree PEG are the same as those in example 5.
Example 7
A mask was prepared in the same procedure and manner as in example 1, except that the prepared dope contained the following components: 2 wt% of silk fibroin, 20 wt% of pullulanase polysaccharide, 0.3 wt% of butanediol and 1.2 wt% of polyglycerol-6 caprylate, wherein the average molecular weight of the silk fibroin is about 40-80KDa, and the molecular weight of the pullulanase polysaccharide is 200000.
Example 8
A mask was prepared in the same procedure and manner as in example 1, except that the prepared dope contained the following components: 12 wt% silk fibroin, 3 wt% sodium hyaluronate, 3.0 wt% pullulanase polysaccharide, 3 wt% maltooligosaccharide glucoside, 2 wt% hydrogenated starch hydrolysate, 1.2 wt% glycerol, 0.8 wt% polyglycerol-6 caprylate, and 0.1 wt% preservative, wherein the average molecular weight of the silk fibroin used is about 40-80KDa, the average molecular weight of the sodium hyaluronate used is about 33000, the average molecular weight of the sodium hyaluronate used is about 39000, and the molecular weight of the pullulanase polysaccharide used is 200000.
Example 9
A mask was prepared in the same procedure and manner as in example 1, except that the prepared dope contained the following components: 15 wt% of silk fibroin, 10 wt% of sodium hyaluronate, 0.3 wt% of PEG with high polymerization degree, 1.3 wt% of PEG with low polymerization degree, 1.0 wt% of ethylene glycol and 1.8 wt% of polyglycerol-6 caprylate, wherein the average molecular weight of the silk fibroin used is about 40-80KDa, the average molecular weight of the sodium hyaluronate used is about 43000, the average molecular weight of the PEG with high polymerization degree is about 230000, and the average molecular weight of the PEG with low polymerization degree is about 7500.
Example 10
The mask was prepared in the same procedure and manner as in example 1, but it was further subjected to a step of forming a peelable protective layer of PE film on top of the spun yarn (nanofiber layer) and removing static electricity. That is, the final face film has three layers, a nonwoven fabric is used as a backing, electrospinning is spun on the nonwoven fabric backing, and the filaments formed by electrospinning are the middle layer (nanofiber layer).
Mask penetration and diffusion efficacy test (Guangdong Boxi Biotech limited company)
The mask prepared by the invention is taken and subjected to a penetration and diffusion efficacy test in Guangdong Boxi biological technology limited company, and the efficacy test compares the penetration and diffusion conditions of the mask solution and the dry mask. The test methods and results are as follows:
1.1 detection method
Differences in efficacy in promoting collagen penetration and skin absorption were assessed using the back skin of suckling pigs based on Franz diffusion cells by testing the penetration behavior of collagen components in the skin ex vivo. The active substance of the nano instant dry facial mask is about 0.12g, when the facial mask is used, the skin on the face needs to be uniformly moistened by water, the water consumption is 5-6 times of pump head extrusion amount of spray pump (about 1g of purified water), and the actual concentration of the nano instant facial mask is about 11% after the nano instant dry facial mask is used according to the method; the concentration of the comparative mask solution in the efficacy test is also 11%. The dry facial mask and the facial mask solution have the same formula and similar use concentration, and the collagen distribution detection is carried out by using the immunofluorescence method after sampling for 0h, 2h, 4h, 6h and 24h of the test products, so that the penetration and diffusion conditions of the two product forms are compared.
1.2 detection System
Piggy back skin with age of 1-2 months
1.3 test materials and devices
TK-12D type drug transdermal absorption Franz diffusion cell (sheath power medicine science Co., Ltd.); constant temperature magnetic stirrer
Description of the drawings: FIG. 1 shows a schematic diagram of diffusion cell operation.
1.4 test results
Fig. 2 and fig. 3 show the variation trend of the analysis result of the fluorescence data of the permeation diffusion experiment, respectively, and the result shows that:
according to the analysis of immunofluorescence results, the samples are mostly concentrated at the stratum corneum part at the beginning of 2h, the samples gradually enter the living cell layer from the stratum corneum after 4h to 6h, and both samples can be seen to enter the dermis after 24 h. In addition, in the whole process, the collagen signal detectable by the silk fibroin collagen nano instant dry facial mask group at the same time point is higher than that of the silk fibroin collagen nano instant facial mask solution, and particularly, the fluorescence signal in the dermis layer of the nano instant dry facial mask group is obviously higher than that of the nano instant facial mask solution in 24 hours. The results show that both samples can promote collagen macromolecular active substances to the dermis, and the nano instant dry facial mask disclosed by the invention has a better effect of promoting the absorption of collagen macromolecules by skin.
Claims (9)
1. The collagen nanometer instant facial mask containing silk fibroin comprises a non-woven fabric base material layer and a nanofiber layer, wherein the nanofiber layer is formed on the non-woven fabric base material layer by adopting an electrostatic spinning method, and the nanofiber layer comprises:
1-30 parts of silk fibroin, preferably 1-20 parts of silk fibroin;
0.1 to 3 parts by weight of a lower polyhydric alcohol; and
0.1 to 5 parts by weight of a surface-active substance;
wherein the average molecular weight of the silk fibroin is 20000-80000, preferably 30000-50000;
wherein the lower polyol is C2-C6The polyol of (1);
wherein the surface active substance is water-soluble, has a skin care effect and is beneficial to electrostatic spinning.
2. The mask pack of claim 1, wherein the nanofiber layer further comprises:
0.1-10 parts by weight of sodium hyaluronate;
wherein the average molecular weight of the sodium hyaluronate is 20000-60000;
wherein the weight ratio of the silk fibroin to the sodium hyaluronate is 100: 1 to 1: 100, preferably between 100: 1 to 10: 100, respectively.
3. The mask pack of claim 1, wherein the nanofiber layer further comprises:
1-25 parts by weight of pullulanase;
wherein the average molecular weight of the pullulanase polysaccharide is 100000-300000;
wherein the weight ratio of the silk fibroin to the pullulanase is 80: 1 to 1: 80, preferably between 80: 3 to 3: 80.
4. The mask pack of claim 1, wherein the nanofiber layer comprises:
1-20 parts by weight of silk fibroin;
0.1-10 parts by weight of sodium hyaluronate;
1-20 parts by weight of pullulanase;
0.2-1 parts by weight of a lower polyhydric alcohol; and
0.1-2 parts by weight of a surface active substance;
wherein the average molecular weight of the used sodium hyaluronate is 20000-60000, and the average molecular weight of the used pullulanase is 100000-300000;
wherein, the silk fibroin: the weight ratio of (sodium hyaluronate + pullulanase) is 60: 1 to 1: 60, preferably between 60: 3 to 3: 60, respectively.
5. The mask pack according to any one of claims 1 to 4, wherein the nanofiber layer further comprises:
0.05-5 parts by weight of maltooligosaccharide glucoside; and
0.03-3 parts by weight of hydrogenated starch hydrolysate.
6. The mask pack according to any one of claims 1 to 4, wherein the nanofiber layer further comprises:
0.1-4 parts by weight of polyethylene glycol having a high degree of polymerization;
0.1 to 2 parts by weight of polyethylene glycol having a low degree of polymerization;
wherein the average molecular weight of the polyethylene glycol with high polymerization degree is 250000-350000, and the average molecular weight of the polyethylene glycol with low polymerization degree is 6000-10000.
7. The mask pack according to any one of claims 1 to 4, wherein the nanofiber layer further comprises:
0.1-10 parts by weight of yeast recombinant collagen;
wherein the average molecular weight of the yeast recombinant collagen is 20000-100000, preferably 40000-80000.
8. A method of preparing a mask pack according to any one of claims 1 to 7, wherein the method comprises the steps of:
(1) and preparing a spinning solution: adding silk fibroin, lower polyhydric alcohol and surface active substances into purified water serving as a solvent, and stirring to form uniform spinning solution, wherein the spinning solution comprises 1-30 wt% of silk fibroin, 0.1-3 wt% of lower polyhydric alcohol and 0.1-5 wt% of surface active substances;
(2) and electrostatic spinning: adding the prepared spinning solution into electrostatic spinning equipment, and carrying out electrostatic spinning by taking non-woven fabrics as a receiving base material;
wherein the average molecular weight of the silk fibroin is 20000-80000, preferably 30000-50000;
wherein the surface active substance is water-soluble, has a skin care effect and is beneficial to electrostatic spinning.
9. The method as claimed in claim 8, wherein the spinning solution further comprises 0.1-10 wt% of sodium hyaluronate or 1-25 wt% of pullulanase polysaccharide, wherein the average molecular weight of the sodium hyaluronate is 20000-60000, and the average molecular weight of the pullulanase polysaccharide is 100000-300000; preferably, the spinning solution further comprises: 0.05-5 wt% of maltooligosaccharide glucoside, 0.03-3 wt% of hydrogenated starch hydrolysate and/or 0.1-4 wt% of polyethylene glycol with high polymerization degree and 0.1-2 wt% of polyethylene glycol with low polymerization degree, wherein the average molecular weight of the polyethylene glycol with high polymerization degree is 250000-350000, and the average molecular weight of the polyethylene glycol with low polymerization degree is 6000-10000.
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| CN115120530A (en) * | 2022-06-20 | 2022-09-30 | 诺斯贝尔化妆品股份有限公司 | Dry instant membrane based on electrostatic spinning and preparation method thereof |
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| CN114795976A (en) * | 2022-05-10 | 2022-07-29 | 中原工学院 | Whitening solid mask compounded by sericin microspheres and fibroin nanofibers and preparation method thereof |
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| CN114948757A (en) * | 2022-06-20 | 2022-08-30 | 诺斯贝尔化妆品股份有限公司 | High-permeability electrostatic spinning dry instant membrane and preparation method thereof |
| CN115120530A (en) * | 2022-06-20 | 2022-09-30 | 诺斯贝尔化妆品股份有限公司 | Dry instant membrane based on electrostatic spinning and preparation method thereof |
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