PEG / HPC nanofiber membrane as well as preparation method and application thereof

PEG and HPC were combined through electrospinning technology to prepare PEG/HPC nanofiber membrane, which solved the problem of low tensile deformation of PEG nanofiber membrane, improved its stress-strain properties, and expanded its application range in the biomedical field.

CN120608367APending Publication Date: 2025-09-09MINJIANG UNIVERSITY
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Patent Information

Application Number
CN202410255989.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-03-06
Publication Date
2025-09-09

AI Technical Summary

Technical Problem

The PEG nanofiber membrane has low tensile deformation, making it difficult to achieve sustained drug release for wound dressings, and its high water solubility limits its application.

Method used

Polyethylene glycol (PEG) and hydroxypropyl cellulose (HPC) were combined by electrospinning technology to prepare PEG/HPC nanofiber membrane, which improved its tensile deformation and stress-strain properties.

Benefits of technology

The tensile deformation of the PEG/HPC nanofiber membrane increased by 20-40%, and the stress increased by 20-40%, broadening its application potential in the biomedical field.

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Abstract

The invention discloses a PEG / HPC nanofiber membrane and a preparation method and application thereof.The preparation method comprises the steps that polyethylene glycol, a solvent and hydroxy propyl cellulose are mixed and subjected to ultrasonic treatment to be uniform, the solvent is removed, a mixed solution is obtained, and the hydroxy propyl cellulose accounts for 1-5 wt% of the polyethylene glycol; the mixed solution is subjected to electrostatic spinning, and the PEG / HPC nanofiber membrane is obtained. According to the preparation method, HPC and PEG are combined, the stress-strain performance of the obtained PEG / HPC nanofiber membrane is improved, and compared with a PEG nanofiber membrane, the stress of the PEG / HPC nanofiber membrane is improved by 20-40%, and the tensile deformation under the same tensile force is improved by 30-50%.
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Description

Technical Field

[0001] The present invention belongs to the technical field of polymer medical materials, and in particular relates to a PEG / HPC nanofiber membrane and a preparation method and application thereof. Background Art

[0002] Polyethylene glycol (PEG) is bio-non-toxic and non-immunogenic, highly flexible, and can be used for surface treatment or bioconjugation. It has good water solubility, and the acidic environment produced by degradation is also conducive to inhibiting bacterial growth. It is a popular biomedical material with good solubility with many organic components and good biocompatibility. The porous structure of PEG nanofiber membrane ensures moisture for hemostasis, gas production and exudate absorption, and provides an environment that promotes wound healing. It has considerable potential in the fields of tissue engineering and wound repair. PEG is a polymer approved by the FDA for use in the human body and is widely used in academic research or commercial products. Although PEG nanofiber membrane has good biocompatibility and is non-toxic, PEG is a water-soluble polymer and is dissolved once it comes into contact with water. It has low tensile deformation and poor ductility, making it difficult to achieve sustained drug release for wound dressings. Summary of the Invention

[0003] In view of the shortcomings of the existing technology, the purpose of the present invention is to provide a method for preparing PEG / HPC nanofiber membrane. The preparation method uses polyethylene glycol (PEG) as a base, adds hydroxypropyl cellulose (HPC) and prepares PEG / HPC nanofiber membrane through electrospinning technology, thereby improving the tensile deformation, solving the pain point of low tensile deformation of PEG nanofiber membrane, and broadening its use in the biomedical field.

[0004] Another object of the present invention is to provide a PEG / HPC nanofiber membrane obtained by the above preparation method.

[0005] Another object of the present invention is to provide the use of the above-mentioned PEG / HPC nanofiber membrane in polymer medical dressings.

[0006] Another object of the present invention is to provide a method for increasing the tensile deformation of polyethylene glycol by using hydroxypropyl cellulose.

[0007] The purpose of the present invention is achieved through the following technical solutions.

[0008] A method for preparing a PEG / HPC nanofiber membrane comprises the following steps:

[0009] Step 1: mixing polyethylene glycol (PEG), a solvent, and hydroxypropyl cellulose (HPC), ultrasonically mixing until uniform, and removing the solvent to obtain a mixed solution, wherein the hydroxypropyl cellulose (HPC) is 1 to 5 wt% of the polyethylene glycol (PEG);

[0010] In step 1, the solvent removal is performed at 50-60° C. under stirring.

[0011] In the above technical solution, the rotation speed of the stirring condition is 200-250 rpm.

[0012] In step 1, the ultrasonication is performed at room temperature for 1 to 2 hours.

[0013] In step 1, the ratio of the mass fraction of the polyethylene glycol (PEG) to the volume fraction of the solvent is 1:(8-12), the unit of the mass fraction is g, and the unit of the volume fraction is mL.

[0014] In step 1, the solvent is anhydrous ethanol.

[0015] In step 1, the ratio of polyethylene glycol (PEG) to hydroxypropyl cellulose (HPC) is preferably 1: (0.03-0.04) by mass.

[0016] Step 2: electrospinning the mixed solution to obtain a PEG / HPC nanofiber membrane.

[0017] In step 2, the feed flow rate of the electrospinning is 0.2 to 1.0 L / h, the horizontal distance between the needle tip of the nozzle and the center of the collecting reel is 10 to 15 cm, and the vertical distance is 8 to 12 cm. The inner diameter of the needle tip is 0.34 mm, the outer diameter of the needle tip is 0.6 mm, and the rotation speed of the collecting drum is 200 to 500 rpm.

[0018] In step 2, the relative humidity of the air during electrospinning is ≤30% RH.

[0019] In step 2, the voltage of the electrospinning is 18 to 22 kV.

[0020] The PEG / HPC nanofiber membrane obtained by the above preparation method.

[0021] A nanofiber membrane comprises polyethylene glycol (PEG) and hydroxypropyl cellulose (HPC), wherein the hydroxypropyl cellulose (HPC) accounts for 1 to 5 wt% of the polyethylene glycol (PEG).

[0022] The above-mentioned PEG / HPC nanofiber membrane / nanofiber membrane is used in polymer medical dressing.

[0023] The use of hydroxypropyl cellulose in increasing the tensile deformation of polyethylene glycol.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] 1. The preparation method of the present invention combines HPC and PEG, improving the stress-strain performance of the resulting PEG / HPC nanofiber membrane. Compared with PEG nanofiber membranes, the stress of PEG / HPC nanofiber membranes is improved by 20-40%, and the tensile deformation under the same tensile force is increased by 30-50%.

[0026] 2. The preparation method of the present invention is simple. PEG and HPC are fully combined under stirring by ultrasound and rotary evaporation, and then prepared by electrostatic spinning. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 These are photos of the PEG nanofiber membrane of Comparative Example 1 and the PEG / HPC nanofiber membranes prepared in Examples 1 to 4 after tensile testing;

[0028] Figure 2 SEM images of the PEG / HPC nanofiber membranes prepared in Examples 1 to 4, (a) is Example 1, (b) is Example 2, (c) is Example 3, and (d) is Example 4;

[0029] Figure 3 FTIR analysis of the PEG / HPC nanofiber membranes prepared in Examples 1 to 5;

[0030] Figure 4 The stress-strain curves of the PEG nanofiber membrane of Comparative Example 1 and the PEG / HPC nanofiber membranes prepared in Examples 1 to 4 are shown. DETAILED DESCRIPTION

[0031] The technical solution of the present invention is further described below with reference to specific embodiments.

[0032] The raw materials in the following examples were purchased from the following sources: anhydrous ethanol (≥99.5%), purchased from Sinopharm Chemical Reagent Co., Ltd.;

[0033] Polyethylene glycol (PEG) was purchased from Yisheng Biotechnology (Shanghai) Co., Ltd.

[0034] Hydroxypropyl cellulose (HPC) was purchased from Nanjing Yejian Pharmaceutical Technology Co., Ltd.

[0035] The instruments and models involved in the following embodiments are as follows:

[0036] Electrospinning machine: JDF05 (Changsha Nayi Instrument Technology Co., Ltd., Changsha, China).

[0037] Stress tester: FSM 128NT (frontier semiconductor Co., Ltd., San Jose, USA).

[0038] Examples 1 to 5

[0039] A method for preparing a PEG / HPC nanofiber membrane comprises the following steps:

[0040] Step 1: Mix polyethylene glycol (PEG), solvent, and hydroxypropyl cellulose (HPC) in a beaker, ultrasonicate at room temperature (25°C) for 1 hour until uniform, and remove the solvent using a rotary evaporator at 60°C and stirring (speed of 250 rpm) to obtain a mixed solution, wherein hydroxypropyl cellulose (HPC) is the X of polyethylene glycol (PEG), the value of X is shown in Table 1, the ratio of the mass fraction of polyethylene glycol (PEG) to the volume fraction of the solvent is 1:10, the unit of mass fraction is g, the unit of volume fraction is mL, and the solvent is anhydrous ethanol;

[0041] Step 2, electrospinning the mixed solution to obtain a PEG / HPC nanofiber membrane, wherein the feed flow rate of electrospinning is 0.5 mL / h, the horizontal distance between the needle tip of the nozzle and the center of the collecting reel is 15 cm, and the vertical distance is 12 cm. The nozzle is an international standard 23G model needle, the inner diameter of the needle tip is 0.34 mm, the outer diameter of the needle tip is 0.6 mm, the rotation speed of the collecting drum is 300 rpm, the relative humidity of the air for electrospinning is 30% RH, and the voltage for electrospinning is 21 kV.

[0042] Table 1

[0043]

[0044]

[0045] Comparative Example 1

[0046] A method for preparing a PEG nanofiber membrane is basically the same as the "method for preparing a PEG / HPC nanofiber membrane" in Example 1, the only difference being that hydroxypropyl cellulose (HPC) is not added in this comparative example.

[0047] The PEG nanofiber membrane of comparative example 1 and the PEG / HPC nanofiber membrane prepared in Examples 1 to 4 were subjected to tensile test using a stress tester, and the stress-strain curves were plotted using Origin. Figure 4 As shown in the photo after tensile test Figure 1 shown. Figure 1 and Figure 4 The PEG nanofiber membrane of Comparative Example 1 is shown in the following order: Figure 1 and Figure 4"PEG"), PEG / HPC nanofiber membrane prepared in Example 1 ( Figure 1 and Figure 4 "1 wt% HPC" in Example 2), the PEG / HPC nanofiber membrane prepared in Example 2 ( Figure 1 and Figure 4 "2.5wt% HPC"), PEG / HPC nanofiber membrane prepared in Example 3 ( Figure 1 and Figure 4 "3.5wt% HPC"), PEG / HPC nanofiber membrane prepared in Example 4 ( Figure 1 and Figure 4 Observe Figure 1 and Figure 4 From the tensile cross-section and tensile deformation of the PEG nanofiber membrane and the PEG / HPC nanofiber membrane, it can be clearly seen that from "PEG", "1wt% HPC", "2.5wt% HPC", "3.5wt% HPC" to "4.5wt% HPC", the tensile cross-section changes from smooth to jagged, and the tensile deformation changes from low to high. The more HPC is added, the greater the tensile deformation. As the addition ratio of HPC increases, the tensile deformation of the PEG / HPC nanofiber membrane is significantly improved. When the HPC addition reaches 4.5wt%, the tensile deformation is 30% higher than that of the PEG nanofiber membrane under the same tension. On the basis of Example 4, an attempt was made to increase the addition ratio of HPC, but the solution reached saturation and could not present a good fiber morphology.

[0048] The diameter of the PEG / HPC nanofiber membranes prepared in Examples 1 to 4 was observed and photographed using a scanning electron microscope (Hitachi SEMTM4000, Hitachi Technology Co., Ltd., Japan). The accelerating voltage was 15 kV. The fiber size distribution was measured using Image-Pro Plus 6.0. The diameter of the PEG / HPC nanofiber membrane was marked as much as possible in the image. The test results are shown in Figure 2. Figure 2As shown. Adding HPC can improve the stress-strain properties of PEG nanofiber membranes. The ductility of PEG nanofiber membranes is very poor. HPC is a crystalline cellulose. Its stress-strain properties can be improved by adding HPC. When the addition amount of HPC is 1wt% and 2.5wt%, the fiber diameter of the PEG / HPC nanofiber membrane is about 700-900nm. As the addition amount of HPC increases to 3.5wt%, the diameter of the PEG / HPC nanofiber membrane increases to 800-1100nm. When the HPC addition amount reaches 4.5wt%, although spinning can be successful, the mixed solution approaches saturation, resulting in poor morphology of the PEG / HPC nanofiber membrane, and HPC cannot be added subsequently. Therefore, adding 3.5wt% of HPC is the optimal parameter.

[0049] The PEG / HPC nanofiber membranes prepared in Examples 1 to 5 were analyzed by FTIR using a Fourier Transform infrared spectroscopy. Figure 3 As shown in the figure, when the HPC addition amount increases from 0.05wt% to more than 1wt%, the peak value at 2900cm -1 The disappearance of the nearby C-H alkyl groups increases the overall polymer flexibility, thereby improving the stress-strain properties.

[0050] The above is an exemplary description of the present invention. It should be noted that, without departing from the core of the present invention, any simple deformation, modification or other equivalent replacement that can be made by other skilled in the art without expending creative labor falls within the scope of protection of the present invention.

Claims

1. A method for preparing a PEG / HPC nanofiber membrane, characterized in that: The following steps are involved: Step 1, mixing polyethylene glycol, a solvent and hydroxypropyl cellulose, ultrasonicating until uniform, removing the solvent to obtain a mixed solution, wherein the hydroxypropyl cellulose is 1 to 5 wt% of the polyethylene glycol; Step 2: electrospinning the mixed solution to obtain a PEG / HPC nanofiber membrane.

2. The preparation method according to claim 1, characterized in that In step 1, the solvent removal is performed at 50-60° C. with stirring; in step 1, the ultrasonication is performed at room temperature for 1-2 h.

3. The preparation method according to claim 1, characterized in that In step 1, the ratio of the mass fraction of the polyethylene glycol to the volume fraction of the solvent is 1:(8-12), the unit of the mass fraction is g, and the unit of the volume fraction is mL.

4. The preparation method according to claim 1, characterized in that In step 1, the solvent is anhydrous ethanol.

5. The preparation method according to claim 1, characterized in that In step 2, the feed flow rate of the electrospinning is 0.2-1.0 L / h, the horizontal distance between the needle tip of the nozzle and the center of the collecting reel is 10-15 cm, the vertical distance is 8-12 cm, and the rotation speed of the collecting roller is 200-500 rpm.

6. The preparation method according to claim 1, characterized in that In step 2, the relative humidity of the air during electrospinning is ≤30% RH; in step 2, the voltage of the electrospinning is 18-22 kV.

7. The PEG / HPC nanofiber membrane obtained by the preparation method according to any one of claims 1 to 6.

8. A nanofiber membrane comprising: Polyethylene glycol and hydroxypropyl cellulose, wherein the hydroxypropyl cellulose accounts for 1 to 5 wt % of the polyethylene glycol.

9. Use of the PEG / HPC nanofiber membrane according to claim 7 / the nanofiber membrane according to claim 8 in polymer medical dressings.

10. The use of hydroxypropyl cellulose in increasing the tensile deformation of polyethylene glycol.

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