Electrostatic spinning instant collagen membrane and preparation method thereof

Abstract

The invention discloses an electrostatic spinning instant collagen membrane and a preparation method thereof. The electrostatic spinning instant collagen membrane comprises the following raw materials in percentage by mass: 40%-80% of a natural high-molecular compound, 5%-40% of collagen, 5%-20% of a film-forming agent and 5%-40% of an instant solvent, the electrostatic spinning instant collagen membrane disclosed by the invention has a rapid dissolving property, and compared with a traditional collagen membrane with a dissolving speed of 2-10 minutes, the collagen membrane disclosed by the invention can be rapidly dissolved within 1-30 seconds; a fluorine-free solvent system is used in the preparation process, a chemical cross-linking agent is not needed, and harmful residues are avoided; meanwhile, under the combined action of the raw materials, the mechanical property of the collagen membrane is improved.

Description

Technical Field

[0001] This invention relates to the field of collagen membrane technology, specifically to an electrospun, rapidly dissolving collagen membrane and its preparation method. Background Technology

[0002] Collagen, as an important natural polymer material, is widely used in medical aesthetic dressings, wound healing, and drug delivery. However, traditional collagen membrane solutions suffer from problems such as slow dissolution rate, insufficient mechanical strength, low preparation efficiency, and poor functional adjustability. In addition, existing electrospun collagen membranes mostly use fluorinated solvents, which pose toxicity and cost issues, and their dissolution rate still cannot meet the requirements for rapid dissolution.

[0003] In view of this, the present invention is hereby proposed. Summary of the Invention

[0004] The purpose of this invention is to provide an electrospun, rapidly dissolving collagen membrane and its preparation method. The electrospun, rapidly dissolving collagen membrane of this invention has rapid dissolution performance, excellent mechanical properties, and is prepared without fluorine solvents, has high biosafety, and can load various functional components to improve the efficacy of the collagen membrane.

[0005] In order to achieve the above-mentioned objectives of the present invention, the following technical solution is adopted:

[0006] The first aspect of this invention provides an electrospun, rapidly dissolving collagen membrane, the electrospun, rapidly dissolving collagen membrane comprising the following raw materials in weight percentages:

[0007] The ingredients include 40%–80% natural polymers, 5%–40% collagen, 5%–20% film-forming agents, and 5%–40% quick-dissolving agents.

[0008] Preferably, the natural polymer compound is selected from at least one of pectin, pectin derivatives, sodium alginate, sodium alginate derivatives, guar gum, and guar gum derivatives.

[0009] Preferably, the collagen is type I collagen or collagen peptide powder.

[0010] Preferably, the film-forming agent is selected from at least one of gelatin, sodium hyaluronate, polyvinylpyrrolidone, and chitosan oligosaccharide.

[0011] Preferably, the instant solvent is selected from at least one of mannitol, sorbitol, erythritol, and soluble oligosaccharides.

[0012] Preferably, the electrospun quick-dissolving collagen membrane further includes 0.1% to 10% of functional components; the functional components are selected from at least one of vitamin C, panthenol, growth factors, small molecule active peptides, antioxidants and Centella asiatica extract.

[0013] A second aspect of the present invention provides a method for preparing the electrospun, rapidly dissolving collagen membrane, the method comprising the following steps:

[0014] (a) Dissolve natural polymers and collagen in a mixed aqueous solution of ethanol and acetic acid, then add a quick-dissolving agent and a film-forming agent and stir for a period of time to obtain a spinning solution;

[0015] (b) Electrospinning the spinning solution to form nanofibers;

[0016] (c) Nanofibers are deposited on a collecting drum to form a nanofiber membrane, which is then dried under vacuum to obtain the electrospun instant collagen membrane.

[0017] Preferably, the volume ratio of acetic acid, ethanol and water in the mixed aqueous solution of ethanol and acetic acid is (5~7)∶((2~4))∶1.

[0018] Preferably, the stirring time is 4 to 12 hours.

[0019] Preferably, the electrospinning process parameters are as follows: voltage 15~22kV, distance 10~18cm, and flow rate 0.2~0.8ml / h.

[0020] Compared with the prior art, the beneficial effects of the present invention include at least the following:

[0021] This invention provides an electrospun, rapidly dissolving collagen membrane with rapid dissolution properties. Compared to the traditional collagen membrane's dissolution rate of 2-10 minutes, this invention's collagen membrane dissolves rapidly within 1-30 seconds. Furthermore, the preparation process uses a fluorine-free solvent system, eliminating the need for chemical cross-linking agents and avoiding harmful residues. Simultaneously, the combined effect of the various raw materials improves the mechanical properties of the collagen membrane. In addition, this invention uses electrospinning to form the collagen membrane, resulting in a uniform structure and controllable thickness, making it suitable for various applications such as medical aesthetic masks and wound dressings. Moreover, the collagen membrane of this invention has a porous structure, allowing it to load various functional components and achieve rapid release of these components. Detailed Implementation

[0022] The embodiments of the technical solution of the present invention will be described in detail below with reference to the examples. The following embodiments are only used to illustrate the technical solution of the present invention more clearly, and are therefore only examples, and should not be used to limit the scope of protection of the present invention.

[0023] It should be noted that, unless otherwise stated, the technical or scientific terms used in this application should have the ordinary meaning as understood by those skilled in the art to which this invention pertains.

[0024] This invention provides an electrospun, rapidly dissolving collagen membrane, which comprises the following raw materials in weight percentages:

[0025] The ingredients include 40%–80% natural polymers, 5%–40% collagen, 5%–20% film-forming agents, and 5%–40% quick-dissolving agents.

[0026] In one embodiment, the natural polymer compound is selected from at least one of pectin, pectin derivatives, sodium alginate, sodium alginate derivatives, guar gum, and guar gum derivatives.

[0027] In one embodiment, the collagen is type I collagen or collagen peptide powder.

[0028] In one embodiment, the film-forming agent is selected from at least one of gelatin, sodium hyaluronate, polyvinylpyrrolidone, and chitosan oligosaccharide.

[0029] In one embodiment, the instant solvent is selected from at least one of mannitol, sorbitol, erythritol, and soluble oligosaccharides.

[0030] In one embodiment, the electrospun quick-dissolving collagen membrane further includes 0.1% to 10% of a functional component; the functional component is selected from at least one of vitamin C, panthenol, growth factors, small molecule active peptides, antioxidants, and centella asiatica extract.

[0031] Another embodiment of the present invention provides a method for preparing the electrospun, rapidly dissolving collagen membrane, the method comprising the following steps:

[0032] (a) Dissolve natural polymers and collagen in a mixed aqueous solution of ethanol and acetic acid, then add a quick-dissolving agent and a film-forming agent and stir for a period of time to obtain a spinning solution;

[0033] (b) Electrospinning the spinning solution to form nanofibers;

[0034] (c) Nanofibers are deposited on a collecting drum to form a nanofiber membrane, which is then dried under vacuum to obtain the electrospun instant collagen membrane.

[0035] In one embodiment, the volume ratio of acetic acid, ethanol and water in the mixed aqueous solution of ethanol and acetic acid is (5~7)∶((2~4))∶1.

[0036] In one embodiment, the stirring time is 4 to 12 hours.

[0037] In one embodiment, the electrospinning process parameters are as follows: voltage 15~22kV, distance 10~18cm, and flow rate 0.2~0.8ml / h.

[0038] The technical solution of the present invention will be further described in detail below through specific embodiments.

[0039] Example 1

[0040] This embodiment is an electrospun, rapidly dissolving collagen membrane, which comprises the following raw materials in the following mass percentages:

[0041] The formula contains 40% natural polymer, 40% collagen, 10% film-forming agent, and 10% quick-dissolving agent. The natural polymer is sodium alginate; the collagen is type I collagen; the film-forming agent is chitosan oligosaccharide; and the quick-dissolving agent is erythritol.

[0042] The above-mentioned method for preparing electrospun, rapidly dissolving collagen membrane includes the following steps:

[0043] (a) Dissolve natural polymers and collagen in a mixed aqueous solution of ethanol and acetic acid, then add a quick-acting solvent and a film-forming agent and stir for 10 hours to obtain a spinning solution, wherein the volume ratio of acetic acid, ethanol and water in the mixed aqueous solution of ethanol and acetic acid is 6:3:1.

[0044] (b) Electrospinning the spinning solution to form nanofibers, wherein the electrospinning process parameters are as follows: voltage 18kV, distance 12cm, flow rate 0.3ml / h;

[0045] (c) Nanofibers are deposited on a collecting drum to form a nanofiber membrane, which is then dried under vacuum to obtain the electrospun instant collagen membrane.

[0046] Example 2

[0047] This embodiment is an electrospun, rapidly dissolving collagen membrane, which comprises the following raw materials in the following mass percentages:

[0048] The formula contains 80% natural polymers, 10% collagen, 5% film-forming agent, and 5% quick-dissolving agent. The natural polymer is pectin; the collagen is type I collagen; the film-forming agent is sodium hyaluronate; and the quick-dissolving agent is mannitol.

[0049] The above-mentioned method for preparing electrospun, rapidly dissolving collagen membrane includes the following steps:

[0050] (a) Dissolve natural polymers and collagen in a mixed aqueous solution of ethanol and acetic acid, then add a quick-acting solvent and a film-forming agent and stir for 8 hours to obtain a spinning solution, wherein the volume ratio of acetic acid, ethanol and water in the mixed aqueous solution of ethanol and acetic acid is 6:3:1.

[0051] (b) Electrospinning the spinning solution to form nanofibers, wherein the electrospinning process parameters are as follows: voltage 20kV, distance 15cm, flow rate 0.5ml / h;

[0052] (c) Nanofibers are deposited on a collecting drum to form a nanofiber membrane, which is then dried under vacuum to obtain the electrospun instant collagen membrane.

[0053] Example 3

[0054] This embodiment is an electrospun, rapidly dissolving collagen membrane, which comprises the following raw materials in the following mass percentages:

[0055] The formula contains 50% natural polymers, 30% collagen, 9% film-forming agent, 10% quick-dissolving agent, and 1% functional components. Among these, the functional components are small molecule active peptides, the natural polymers are sodium alginate, the collagen is type I collagen, the film-forming agent is chitosan oligosaccharide, and the quick-dissolving agent is mannitol.

[0056] The above-mentioned method for preparing electrospun, rapidly dissolving collagen membrane includes the following steps:

[0057] (a) Dissolve natural polymers and collagen in a mixed aqueous solution of ethanol and acetic acid, then add a quick-dissolving agent, functional components and film-forming agent and stir for 8 hours to obtain a spinning solution, wherein the volume ratio of acetic acid, ethanol and water in the mixed aqueous solution of ethanol and acetic acid is 6:3:1.

[0058] (b) Electrospinning the spinning solution to form nanofibers, wherein the electrospinning process parameters are as follows: voltage 22kV, distance 16cm, flow rate 0.4ml / h;

[0059] (c) Nanofibers are deposited on a collecting drum to form a nanofiber membrane, which is then dried under vacuum to obtain the electrospun instant collagen membrane.

[0060] Example 4

[0061] This embodiment is an electrospun, rapidly dissolving collagen membrane, which comprises the following raw materials in the following mass percentages:

[0062] The formula contains 40% natural polymer, 40% collagen, 10% film-forming agent, and 10% quick-dissolving agent. The natural polymer is sodium alginate; the collagen is type I collagen; the film-forming agent is chitosan oligosaccharide; and the quick-dissolving agent is mannitol.

[0063] The above-mentioned method for preparing electrospun, rapidly dissolving collagen membrane includes the following steps:

[0064] (a) Dissolve natural polymers and collagen in a mixed aqueous solution of ethanol and acetic acid, then add a quick-acting solvent and a film-forming agent and stir for 10 hours to obtain a spinning solution, wherein the volume ratio of acetic acid, ethanol and water in the mixed aqueous solution of ethanol and acetic acid is 6:3:1.

[0065] (b) Electrospinning the spinning solution to form nanofibers, wherein the electrospinning process parameters are as follows: voltage 18kV, distance 12cm, flow rate 0.3ml / h;

[0066] (c) Nanofibers are deposited on a collecting drum to form a nanofiber membrane, which is then dried under vacuum to obtain the electrospun instant collagen membrane.

[0067] Comparative Example 1

[0068] This comparative example is an electrospun, rapidly dissolving collagen membrane, which comprises the following raw materials in the following mass percentages:

[0069] The formula contains 40% natural polymers, 50% collagen, and 10% film-forming agents. The natural polymer is sodium alginate; the collagen is type I collagen; and the film-forming agent is chitosan oligosaccharide.

[0070] The above-mentioned method for preparing electrospun, rapidly dissolving collagen membrane includes the following steps:

[0071] (a) Dissolve natural polymers and collagen in a mixed aqueous solution of ethanol and acetic acid, add a film-forming agent and stir for 10 h to obtain a spinning solution, wherein the volume ratio of acetic acid, ethanol and water in the mixed aqueous solution of ethanol and acetic acid is 6:3:1.

[0072] (b) Electrospinning the spinning solution to form nanofibers, wherein the electrospinning process parameters are as follows: voltage 18kV, distance 12cm, flow rate 0.3ml / h;

[0073] (c) Nanofibers are deposited on a collecting drum to form a nanofiber membrane, which is then dried under vacuum to obtain the electrospun instant collagen membrane.

[0074] Experimental Example

[0075] Electrospun fast-dissolving collagen membranes (0.5 mm thick) from Examples 1, 4 and Comparative Example 1 were obtained respectively.

[0076] The electrospun, rapidly dissolving collagen membrane described above was placed in water, and the time required for complete dissolution (2 cm) was measured. 2 The tensile strength of the layers was measured; the results are shown in Table 1.

[0077] Table 1

[0078] Group Time (s) Tensile strength (MPa) Example 1 7 2.7 Example 4 3 2.4 Comparative Example 1 36 1.9

[0079] As shown in Table 1:

[0080] Compared with the comparative example, the electrospun fast-dissolving collagen membrane prepared in the embodiments of the present invention has a faster dissolution rate and better mechanical properties.

[0081] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention, and they should all be covered within the scope of the claims and specification of the present invention.

Claims

1. An electrospun fast dissolving collagen protein film, characterized in that, The electrospinning fast-dissolving collagen membrane comprises raw materials in the following mass percentages: 40-80% of a natural polymer compound, 5-40% of collagen, 5-20% of a film-forming agent, and 5-40% of a fast-dissolving agent.

2. The electrospun fast dissolving collagen protein film according to claim 1, wherein, The natural polymer compound is at least one selected from the group consisting of pectin, a pectin derivative, sodium alginate, a sodium alginate derivative, guar gum, and a guar gum derivative.

3. The electrospun fast dissolving collagen protein film of claim 1, wherein, The collagen is type I collagen or collagen peptide powder.

4. The electrospun fast dissolving collagen protein film of claim 1, wherein, The film-forming agent is at least one selected from the group consisting of gelatin, sodium hyaluronate, polyvinylpyrrolidone, and chitosan oligosaccharide.

5. The electrospun fast dissolving collagen protein film of claim 1, wherein, The fast-dissolving agent is at least one selected from the group consisting of mannitol, sorbitol, erythritol, and soluble oligosaccharide.

6. The electrospun fast dissolving collagen protein film of claim 1, wherein, The electrospinning fast-dissolving collagen membrane further comprises 0.1-10% of a functional component; the functional component is at least one selected from the group consisting of vitamin C, panthenol, a growth factor, a small-molecule active peptide, an antioxidant, and an extract of Gynostemma pentaphyllum.

7. The method of producing an electrospun fast dissolving collagen protein film according to any one of claims 1 to 6, characterized in that, The preparation method comprises the following steps: (a) dissolving the natural polymer compound and the collagen in a mixed aqueous solution of ethanol and acetic acid, then adding the fast-dissolving agent and the film-forming agent and stirring for a period of time to obtain a spinning solution; (b) electrospinning the spinning solution to form nanofibers; (c) depositing the nanofibers on a collection drum to form a nanofiber membrane, and then vacuum drying to obtain the electrospinning fast-dissolving collagen membrane.

8. The method of claim 1, wherein, The volume ratio of acetic acid, ethanol, and water in the mixed aqueous solution of ethanol and acetic acid is (5-7):(2-4):

1.

9. The method of claim 1, wherein, The stirring for a period of time is 4-12 hours.

10. The method of claim 1, wherein, The electrospinning process parameters are as follows: voltage 15-22 kV, distance 10-18 cm, and flow rate 0.2-0.8 ml / h.