Shell-core nanofiber membrane with temperature-controlled shrinkage, preparation method and application thereof

Abstract

The present application relates to a kind of shell-core nanofiber membrane with temperature control shrinkage, preparation method and application;DCM and DMF are sequentially added to the mixture consisting of PTMC and PVP to obtain a mixed solution, wherein the mass percentage of solute is 2-5%; the mixed solution is stirred to obtain an electrospinning precursor solution after sufficient dissolution;After electrospinning of electrospinning precursor solution using single shaft spinneret, vacuum drying obtains nanofiber membrane, the fiber diameter of the nanofiber membrane is 0.203-0.603 μm, has shrinkage under humid conditions, and the shrinkage is enhanced with the increase of temperature, and the shrinkage rate in PBS at 20 DEG C to 37 DEG C for 2h is 20.4% to 54.33%; the nanofiber membrane adheres to wound site can effectively reduce wound area, for promoting active healing of wound, using single shaft electrospinning process preparation, it is more simple and convenient, more economical to operate.

Description

Technical Field

[0001] This invention belongs to the field of biomaterials technology, specifically relating to a shell-core nanofiber membrane with temperature-controlled shrinkage, its preparation method, and its application. Specifically, it is prepared using uniaxial electrospinning technology and is used to promote wound healing. Background Technology

[0002] Skin injuries impair the integrity and protective function of the skin. Covering exposed wounds with dressings is a common clinical wound care method. During the natural healing process of a skin wound, 2-3 days after injury, myofibroblasts pull the entire layer of skin and subcutaneous tissue towards the center, causing the wound to shrink rapidly. This wound contraction is significant in reducing the wound area and promoting healing. Traditional wound dressings cannot meet the needs of accelerating wound shrinkage and promoting active wound healing.

[0003] The traditional process for preparing shell-core nanofibers is coaxial electrospinning, which requires complex equipment and precise parameter adjustments. Compared to coaxial electrospinning, uniaxial electrospinning is a more economical and simpler method for preparing shell-core nanofibers.

[0004] Polyvinylpyrrolidone (PVP) is a water-soluble polymer compound with good biocompatibility, hygroscopicity, and adhesive properties, and is widely used in the biomedical field. However, electrospun PVP nanofiber membranes have poor mechanical properties. In addition, because PVP is highly soluble in water, it is difficult to maintain the shape and structure of dressings when in contact with moist wounds. Therefore, its properties are often improved by blending with other polymers and electrospinning.

[0005] Polytrimethylene carbonate (PTMC) is a biodegradable amorphous polymer with good biocompatibility and mechanical properties. It possesses unique degradation characteristics, including resistance to non-enzymatic and surface degradation mechanisms, which allows PTMC to maintain structural stability during degradation. Furthermore, its degradation products are neutral, avoiding the inflammatory irritation to wounds caused by acidic degradation products. Experiments have shown that PTMC nanofiber membranes prepared by electrospinning exhibit shrinkage under humid conditions, and this shrinkage increases with increasing temperature. However, the poor adhesion and hydrophilicity of PTMC limit its application as a wound dressing. Summary of the Invention

[0006] The purpose of this invention is to provide a shell-core nanofiber membrane with temperature-controlled shrinkage. This nanofiber membrane exhibits shrinkage under humid conditions, and its shrinkage increases with increasing temperature. When this nanofiber membrane adheres to a wound, it can effectively reduce the wound area and promote active wound healing. This nanofiber membrane is prepared using a uniaxial electrospinning process, which is simpler and more economical to operate.

[0007] The objective of this invention is achieved through the following technical solution:

[0008] A shell-core nanofiber membrane with temperature-controlled shrinkage is prepared by the following method:

[0009] Step 1: Add DCM and DMF sequentially to the mixture composed of PTMC and PVP to obtain a mixed solution, wherein the mass percentage of solute is 2-5%;

[0010] Step 2: Stir the mixed solution until fully dissolved to obtain an electrospinning precursor solution;

[0011] Step 3: Electrospin the electrospinning precursor solution using a uniaxial spinneret, and obtain a nanofiber membrane after vacuum drying.

[0012] As a preferred technical solution of the present invention, the vacuum drying time of the nanofiber membrane is 18-30 hours.

[0013] As a preferred technical solution of the present invention, the mass ratio of PTMC to PVP in the electrospinning precursor solution is 1:5 to 3:1, and the mass ratio of DCM to DMF is 2:1 to 4:1.

[0014] As a preferred technical solution of the present invention, the mass ratio of PTMC to PVP in the electrospinning precursor solution is 1:3, and the mass ratio of DCM to DMF is 3:1.

[0015] As a preferred technical solution of the present invention, the electrospinning parameters are: voltage 13-18kV, feed rate 1-2.5ml / h, distance from spinneret to collecting plate 15-25cm, and needle inner diameter 21G.

[0016] As a preferred technical solution of the present invention, the electrospinning parameters are: voltage 15kv, feed rate 2ml / h, distance from spinneret to collecting plate 20cm, and needle inner diameter 21G.

[0017] As a preferred technical solution of the present invention, the mass percentage of the solute is 3%.

[0018] As a preferred technical solution of the present invention, the nanofiber membrane is vacuum dried for 24 hours.

[0019] Another objective of this invention is to provide an application of a shell-core nanofiber membrane with temperature-controlled shrinkage in promoting wound healing.

[0020] The beneficial effects are as follows:

[0021] The nanofiber membrane of the present invention has a fiber diameter of 0.203–0.603 μm and exhibits good biocompatibility; it is shrinkable under humid conditions, and its shrinkage increases with increasing temperature, with a shrinkage rate of 20.4%–54.33% after 2 hours in PBS at 20°C to 37°C; it can reduce the wound area when adhered to the wound site, thereby promoting active wound healing; it can also achieve good adhesion to the skin, preventing dressing from falling off.

[0022] This invention uses a uniaxial electrospinning process to prepare shell-core nanofibers, which has the advantages of simple process, easy operation, low cost and easy industrial production, and has a wide range of application prospects.

[0023] The nanofiber membrane of this invention achieves the goal of promoting active wound healing. Attached Figure Description

[0024] Figure 1 This is a scanning electron microscope image of the nanofiber membrane prepared in Example 1 of the present invention;

[0025] Figure 2 This is a transmission electron microscope image of the nanofiber membrane prepared in Example 1 of the present invention;

[0026] Figure 3 This is a nitrogen element distribution diagram of the nanofiber membrane prepared in Example 1 of the present invention;

[0027] Figure 4 The images show the in vitro shrinkage of the nanofiber membranes prepared in Examples 1 to 3 of this invention after being immersed in PBS solutions at 20°C and 37°C for 2 hours.

[0028] Figure 5 To illustrate the changes in wound area before and after applying the nanofiber membrane prepared in Example 1 of this invention to a skin defect in a rat and placing it at 37°C for 30 minutes, the image shows the changes in wound area before and after application. Detailed Implementation

[0029] The technical solution of the present invention will be further described in detail below with reference to the embodiments.

[0030] All raw materials used in this invention are commercially available.

[0031] All ranges described throughout this specification include all values ​​and subranges therein, unless otherwise stated.

[0032] Example 1

[0033] Step 1: Add 8.73g DCM and 2.91g DMF sequentially to a mixture consisting of 0.09g PTMC and 0.27g PVP to obtain a mixed solution, wherein the mass percentage of the solute is 3%.

[0034] Step 2: Stir the mixed solution until fully dissolved to obtain an electrospinning precursor solution.

[0035] Step 3: Electrospin the electrospinning precursor solution using a uniaxial spinneret to obtain a nanofiber membrane. The electrospinning parameters are: voltage 15kV, feed rate 2ml / h, distance from the spinneret to the collecting plate 20cm, and needle inner diameter 21G.

[0036] Step 4: Vacuum dry the nanofiber membrane for 24 hours.

[0037] Example 2

[0038] The difference between this embodiment and embodiment 1 is that the mass of PTMC added in step one is 0.18g, the mass of PVP is 0.18g, and other process conditions are the same as in embodiment 1.

[0039] Example 3

[0040] The difference between this embodiment and Embodiment 1 is that the mass of PTMC added in step one is 0.27g, the mass of PVP is 0.09g, and all other process conditions are the same as in Embodiment 1.

[0041] Example 4

[0042] The difference between this embodiment and Embodiment 1 is that the mass of PTMC added in step one is 0.06g, the mass of PVP is 0.3g, and all other process conditions are the same as in Embodiment 1.

[0043] Example 5

[0044] The difference between this embodiment and Embodiment 1 is that the mass of DCM added in step one is 9.312g, the mass of DMF is 2.328g, and all other process conditions are the same as in Embodiment 1.

[0045] Example 6

[0046] The difference between this embodiment and embodiment 1 is that the mass of DCM added in step one is 7.76g and the mass of DMF is 3.88g, while other process conditions are the same as in embodiment 1.

[0047] Example 7

[0048] The difference between this embodiment and Embodiment 1 is that the mass percentage of the solute in step one is 2%, that is, the mass of added DCM is 8.64g, the mass of DMF is 2.88g, the mass of PTMC is 0.12g, and the mass of PVP is 0.36g. All other process conditions are the same as in Embodiment 1.

[0049] Example 8

[0050] The difference between this embodiment and Embodiment 1 is that the mass percentage of the solute in step one is 5%, that is, the mass of added DCM is 8.46g, the mass of DMF is 2.82g, the mass of PTMC is 0.18g, and the mass of PVP is 0.54g. All other process conditions are the same as in Embodiment 1.

[0051] Example 9

[0052] The difference between this embodiment and Embodiment 1 is that the electrospinning parameters in step three are the same as in Embodiment 1, with a voltage of 13kV.

[0053] Example 10

[0054] The difference between this embodiment and Embodiment 1 is that the electrospinning parameters in step three are the same as in Embodiment 1, with a voltage of 18kV.

[0055] Example 11

[0056] The difference between this embodiment and Embodiment 1 is that the electrospinning parameters in step three are the same as in Embodiment 1, with the solution feed rate being 1 ml / h.

[0057] Example 12

[0058] The difference between this embodiment and Embodiment 1 is that the electrospinning parameters in step three are as follows: the solution feed rate is 2.5 ml / h, and all other process conditions are the same as in Embodiment 1.

[0059] Example 13

[0060] The difference between this embodiment and Embodiment 1 is that the electrospinning parameters in step three have a distance of 15cm from the spinneret to the collecting plate, while other process conditions are the same as in Embodiment 1.

[0061] Example 14

[0062] The difference between this embodiment and Embodiment 1 is that the electrospinning parameters in step three are as follows: the distance from the spinneret to the collecting plate is 25cm, and all other process conditions are the same as in Embodiment 1.

[0063] Example 15

[0064] The difference between this embodiment and Embodiment 1 is that the obtained nanofiber membrane is vacuum dried for 18 hours in step four, while other process conditions are the same as in Embodiment 1.

[0065] Example 16

[0066] The difference between this embodiment and Embodiment 1 is that the obtained nanofiber membrane is vacuum dried for 30 hours in step four, while other process conditions are the same as in Embodiment 1.

[0067] The morphology of the nanofiber membranes prepared in Examples 1 to 16 was studied using cold field emission scanning electron microscopy, showing that the obtained nanofibers have a porous, beaded structure. The diameters of the nanofibers and beaded structures prepared in Examples 1 to 16 are shown in Table 1. The nanofibers obtained in Example 1 exhibit the best porous, beaded structure. Figure 1 As shown.

[0068] The internal morphology of the nanofiber membranes prepared in Examples 1 to 16 was studied using field emission transmission electron microscopy, showing that the obtained nanofibers possess a shell-core structure. The ratio of the shell to the core diameter of the nanofibers prepared in Examples 1 to 16 is shown in Table 1. The nanofibers obtained in Example 1 exhibit the best shell-core structure. Figure 2 As shown.

[0069] The nitrogen element distribution of the nanofiber membranes prepared in Examples 1 to 16 was analyzed using cold field emission scanning electron microscopy, showing that the nitrogen element in the nanofibers was mainly distributed within the beaded and core structures of the fibers. Figure 3 As shown, the nitrogen element in the nanofibers prepared in Example 1 is mainly distributed in the beaded structure and core structure of the fibers.

[0070] The nanofiber membranes obtained in Examples 1 to 16 were immersed in PBS at 20°C and 37°C for 2 hours. The shrinkage properties of the samples at different temperatures were tested to verify the effect of changes in preparation parameters on nanofibers. The specific shrinkage rates of the nanofibers prepared in Examples 1 to 16 are shown in Table 1.

[0071] Table 1

[0072]

[0073]

[0074] like Figure 4 As shown, the nanofiber membranes obtained in Examples 1, 2 and 3 exhibited greater shrinkage at 37°C than at 20°C.

[0075] The nanofiber membrane obtained in Example 1 was adhered to the skin defect of a rat and placed at 37°C for 30 minutes to test the effect of the sample on wound healing. Figure 5 The nanofiber membrane showed that it reduced the area of ​​skin defects in rats to approximately 80%.

[0076] The above description is merely a preferred embodiment of the present invention, and the scope of protection of the present invention is not limited thereto. Any simple changes or equivalent substitutions of the technical solutions that can be obviously obtained by those skilled in the art within the scope of the technology disclosed in the present invention shall fall within the scope of protection of the present invention.

Claims

1. A method for preparing a shell-core nanofiber membrane with temperature-controlled shrinkage, characterized in that, Includes the following steps: Step 1: Add DCM and DMF sequentially to the mixture composed of PTMC and PVP to obtain a mixed solution, wherein the mass percentage of solute is 2-5%; Step 2: Stir the mixed solution until fully dissolved to obtain an electrospinning precursor solution; Step 3: Electrospin the electrospinning precursor solution using a uniaxial spinneret, and obtain a nanofiber membrane after vacuum drying.

2. The method for preparing a shell-core nanofiber membrane with temperature-controlled shrinkage as described in claim 1, characterized in that, The vacuum drying time of the nanofiber membrane is 18–30 h.

3. The method for preparing a shell-core nanofiber membrane with temperature-controlled shrinkage as described in claim 1, characterized in that, The mass ratio of PTMC to PVP in the electrospinning precursor solution is 1:5 to 3:1, and the mass ratio of DCM to DMF is 2:1 to 4:

1.

4. The method for preparing a shell-core nanofiber membrane with temperature-controlled shrinkage as described in claim 1, characterized in that, The mass ratio of PTMC to PVP in the electrospinning precursor solution is 1:3, and the mass ratio of DCM to DMF is 3:

1.

5. The method for preparing a shell-core nanofiber membrane with temperature-controlled shrinkage as described in claim 1, characterized in that, The electrospinning parameters are as follows: voltage 13-18kV, feed rate 1-2.5mL / h, distance from spinneret to collecting plate 15-25cm, and needle inner diameter 21G.

6. The method for preparing a shell-core nanofiber membrane with temperature-controlled shrinkage as described in claim 1, characterized in that, The electrospinning parameters are as follows: voltage 15kV, feed rate 2mL / h, distance from spinneret to collecting plate 20cm, and needle inner diameter 21G.

7. The method for preparing a shell-core nanofiber membrane with temperature-controlled shrinkage as described in claim 1, characterized in that, The nanofiber membrane was vacuum dried for 24 hours.

8. A shell-core nanofiber membrane with temperature-controlled shrinkage, characterized in that: The shell-core nanofiber membrane is obtained by the method for preparing a temperature-controlled shrinkage shell-core nanofiber membrane as described in any one of claims 1-7.

9. The shell-core nanofiber membrane with temperature-controlled shrinkage as described in claim 8, characterized in that: The application of the shell-core nanofiber membrane in promoting wound healing.

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