Collagen / PVA hydrogel wound dressing as well as preparation method and application thereof
By combining collagen, PVA, borax, hydroxypropyl methylcellulose and polyhexamethylene biguanide, a hydrogel wound dressing with antibacterial and healing-promoting properties was prepared, which solved the problem of wound dressing being easily infected and achieved efficient wound healing effect.
Patent Information
- Application Number
- CN202410443914.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-04-14
- Publication Date
- 2025-10-21
AI Technical Summary
Existing wound dressings lack antibacterial properties and are prone to causing wound infection, and traditional hydrogels have limited effectiveness in promoting healing.
Using collagen, PVA, borax, hydroxypropyl methylcellulose and polyhexamethylene biguanide as raw materials, a hydrogel with a dynamic double network structure was prepared by forming borate bonds and electrostatic interactions, giving it antibacterial and healing-promoting properties.
The prepared hydrogel has good tissue adhesion, rapid self-healing, ultra-stretchability and broad-spectrum antibacterial properties, is low-cost and easy to industrialize.
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Abstract
Description
Technical field:
[0001] The present invention belongs to the field of biomedical materials, and more specifically, relates to a collagen / PVA hydrogel wound dressing and a preparation method and application thereof. Background technology:
[0002] The skin is a very important organ that covers the surface of the human body and is in direct contact with the external environment. The repair of skin wounds is a complex and orderly process. Hydrogels are three-dimensional networks composed of cross-linked hydrophilic polymers with a large number of polar functional groups. Due to their high water content, good biocompatibility, ability to absorb exudates, ease of removal, and provision of a moist environment, they are widely used in the field of wound dressings. Traditional wound dressings have a protective effect on wounds, but lack antibacterial properties and can easily cause wound infection. The new hydrogel wound dressing can play an excellent role in promoting healing during wound treatment, acting as a barrier to directly protect wounds and prevent bacterial and fungal infections or secondary trauma.
[0003] Collagen is a natural high-molecular-weight protein widely found in animal connective tissue and is a key raw material in the biotechnology field. It is rich in amino acids such as glycine, proline, and hydroxyproline, which are essential to the human body. Collagen is the most important component of the extracellular matrix. Due to its excellent biocompatibility, bioactivity, and biodegradability, hydrogels made from collagen have a stronger affinity for human skin wounds than other materials, are less likely to trigger inflammatory responses, and promote wound healing. They occupy a key position in the field of wound dressings and are currently widely used in the pharmaceutical, cosmetic, food, and chemical industries.
[0004] Polyvinyl alcohol (PVA) is a hydrophilic and film-forming polymer, making it a promising biomaterial suitable for tissue simulation, vascular cell culture, and vascular implantation. It is also a widely used water-soluble polymer with excellent water solubility, is non-toxic, odorless, and non-irritating to the skin, without causing skin allergies. Borax is a very important boron-containing mineral and boron compound with a wide range of uses, including as a detergent, cosmetics, and pesticide, as well as for preparing buffer solutions and preparing other boron compounds. Borax can also serve as a crosslinker, forming boric acid diester bonds with PVA to form soft, stretchable hydrogels.
[0005] Hydroxypropyl methylcellulose (HPMC), also known as hydroxypropyl methylcellulose, is a nonionic cellulose ether. It is a semisynthetic, inactive, viscoelastic polymer commonly used as a lubricant in ophthalmology and as an excipient or excipient in oral medications. It has the advantages of low toxicity, high biocompatibility, and good viscoelasticity. It can be used as a hydrogel thickener to increase hydrogel stability and support, while also imparting good tissue adhesion.
[0006] Inflammation is the second stage of wound healing, and its main function is to destroy bacteria and remove debris. Appropriate inflammation is crucial in the wound healing process. However, bacterial infection is one of the most common and unavoidable challenges in the wound healing process. The preparation of antibacterial hydrogel dressings has become a hot topic. Polyhexamethylene biguanide (PHMB) is an environmentally friendly polymer bactericidal disinfectant with broad-spectrum bactericidal properties and good sterilization effect. It has a low effective concentration, a fast action speed, and stable performance. It is easily soluble in water and can be used at room temperature. It can inhibit bacteria for a long time, has no toxic side effects, is non-corrosive, colorless, odorless, non-toxic, moderately priced, and easy to transport. It is an excellent antibacterial agent with extremely wide applications in industry, agriculture, medicine, and daily life. Summary of the invention:
[0007] In response to the problems existing in the prior art, the technical problem to be solved by the present invention is to quickly prepare a hydrogel wound dressing with cyclic plasticity, rapid self-healing, super stretchability, dynamic adhesion and antibacterial properties using collagen, PVA, borax, hydroxypropyl methylcellulose and polyhexamethylene biguanide as raw materials, and its application.
[0008] The technical solution adopted by the present invention to solve its technical problem is: the present invention provides a collagen / PVA hydrogel wound dressing, in which the mass percentage concentrations of each component, collagen, PVA, borax, hydroxypropyl methylcellulose, and polyhexamethylene biguanide, are as follows: 0.5-3%, 2-10%, 2-6%, 1.5-2%, and 0.05-0.15%.
[0009] Specifically, the preparation method of the collagen / PVA hydrogel wound dressing is prepared according to the following steps:
[0010] Step 1: Prepare a certain concentration of PBS solution with a pH of 7.4, a certain concentration of NaOH solution, and a 0.5 M glacial acetic acid solution.
[0011] Step 2: Dissolve collagen in glacial acetic acid and adjust the pH to 7-7.4 with PBS and NaOH to obtain a 40% collagen stock solution. Then, weigh PVA and borax solids and dissolve them in water to prepare stock solutions with a concentration of 25%.
[0012] Step 3: Prepare a polyhexamethylene biguanide stock solution with a concentration of 1%.
[0013] Step 4: Add a certain amount of water to the PVA mother liquor and carboxymethyl propyl cellulose powder in a certain proportion and mix them evenly. After the two substances are completely mixed, stir them at 80°C for 15 minutes (heating in a water bath), cool the solution to room temperature, add a certain volume of collagen mother liquor and polyhexamethylene biguanide mother liquor and mix them evenly to form precursor solution I.
[0014] Step 5: Use borax solution as precursor solution II.
[0015] Step 6: The precursor solution I and the precursor solution II described in step 4 and step 5 are uniformly mixed in a certain volume ratio using a vortex mixer to form a hydrogel wound dressing, wherein the mass percentages of collagen, PVA, borax, hydroxymethylpropyl cellulose, and polyhexamethylene biguanide are 0.5-3%, 2-10%, 2-6%, 1.5-2%, and 0.05-0.15%, respectively.
[0016] The invention provides a collagen / PVA hydrogel wound dressing.
[0017] The present invention provides a collagen / PVA hydrogel wound dressing for use as a hydrogel membrane in healing infectious irregular wounds and joint wounds.
[0018] Compared with the prior art, the present invention has the following beneficial effects:
[0019] The present invention uses collagen, PVA, borax, hydroxymethylpropyl cellulose and polyhexamethylene biguanide as raw materials, and forms a dynamic double network structure through the formation of borate bonds and electrostatic interactions to obtain a hydrogel; the hydrogel has good tissue adhesion, cyclic plasticity, rapid self-healing properties, and super stretchability, and can be used as a wound dressing; the polyhexamethylene biguanide contained in the present invention gives the hydrogel broad-spectrum antibacterial properties; the preparation method of the present invention is low-cost, simple and easy to operate, and can be industrialized. Description of the drawings:
[0020] Figure 1 Graph showing tissue adhesion of the hydrogel wound dressing of the present invention.
[0021] Figure 2 This is a diagram showing the stretching and self-healing of the hydrogel wound dressing of the present invention.
[0022] Figure 3 This is a plasticity diagram of the hydrogel wound dressing of the present invention.
[0023] Figure 4 This is the antibacterial property of the hydrogel wound dressing of the present invention. Specific implementation method:
[0024] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.
[0025] Example 1
[0026] A collagen / PVA hydrogel wound dressing was prepared, and the specific implementation method is as follows:
[0027] Step 1: Prepare pH 7.4 PBS solution, 10% NaOH solution and 0.5 M glacial acetic acid solution.
[0028] Step 2: Dissolve collagen in glacial acetic acid and adjust the pH to 7-7.4 with PBS and NaOH to obtain a 40% collagen stock solution. Then, weigh PVA and borax solids and dissolve them in water to prepare stock solutions with a concentration of 25%.
[0029] Step 3: Prepare a polyhexamethylene biguanide stock solution with a concentration of 1%.
[0030] Step 4: Add 500 μL of water to 400 μL of PVA mother liquor and 0.035 g of carboxymethyl propyl cellulose powder and mix well. After the two substances are completely mixed, stir at 80°C for 15 minutes (heat in a water bath), cool the solution to room temperature, add 250 μL of collagen mother liquor and 200 μL of polyhexamethylene biguanide mother liquor, mix well, and add water to a total volume of 1680 μL to form precursor solution I.
[0031] Step 5: Use borax solution as precursor solution II.
[0032] Step 6: The precursor solution I and the precursor solution II described in steps 4 and 5 are mixed in a volume ratio of 21:4, and uniformly mixed using a vortex mixer to form a hydrogel wound dressing, wherein the mass percentages of collagen, PVA, borax, hydroxymethylpropyl cellulose, and polyhexamethylene biguanide are 2.5%, 5%, 4%, 1.75%, and 0.1%, respectively.
[0033] Example 2
[0034] A collagen / PVA hydrogel wound dressing was prepared, and the specific implementation method is as follows:
[0035] Step 1: Prepare pH 7.4 PBS solution, 10% NaOH solution and 0.5 M glacial acetic acid solution.
[0036] Step 2: Dissolve collagen in glacial acetic acid and adjust the pH to 7-7.4 with PBS and NaOH to obtain a 40% collagen stock solution. Then, weigh PVA and borax solids and dissolve them in water to prepare stock solutions with a concentration of 25%.
[0037] Step 3: Prepare a polyhexamethylene biguanide stock solution with a concentration of 1%.
[0038] Step 4: Add 500 μL of water to 400 μL of PVA mother solution and mix evenly. After the two substances are completely mixed, stir at 80°C for 15 minutes (heat in a water bath), cool the solution to room temperature, add 250 μL of collagen mother solution and 200 μL of polyhexamethylene biguanide mother solution, add water to 1680 μL and mix evenly to form precursor solution I.
[0039] Step 5: Use borax solution as precursor solution II.
[0040] Step 6: The precursor solution I and the precursor solution II described in steps 4 and 5 are mixed in a volume ratio of 21:4, and uniformly mixed using a vortex mixer to form a hydrogel wound dressing, wherein the mass percentages of collagen, PVA, borax, and polyhexamethylene biguanide are 2.5%, 5%, 4%, and 0.1%, respectively.
[0041] Example 3
[0042] A collagen / PVA hydrogel wound dressing was prepared, and the specific implementation method is as follows:
[0043] Step 1: Prepare pH 7.4 PBS solution, 10% NaOH solution and 0.5 M glacial acetic acid solution.
[0044] Step 2: Dissolve collagen in glacial acetic acid and adjust the pH to 7-7.4 with PBS and NaOH to obtain a 40% collagen stock solution. Then, weigh PVA and borax solids and dissolve them in water to prepare stock solutions with a concentration of 25%.
[0045] Step 3: Add 500 μL of water to 400 μL of PVA mother liquor and 0.035 g of carboxymethyl propyl cellulose powder and mix evenly. After the two substances are completely mixed, stir at 80°C for 15 minutes (heat in a water bath), cool the solution to room temperature, add 250 μL of collagen mother liquor and mix evenly, and add water to a total volume of 1680 μL to form precursor solution I.
[0046] Step 4: Use borax solution as precursor solution II.
[0047] Step 5: The precursor solution I and the precursor solution II described in steps 3 and 4 are mixed in a volume ratio of 21:4, and uniformly mixed using a vortex mixer to form a hydrogel wound dressing, wherein the mass percentages of collagen, PVA, borax, and hydroxymethylpropyl cellulose are 2.5%, 5%, 6%, and 1.75%, respectively.
[0048] Example 4
[0049] This example was carried out using the product prepared in Example 1.
[0050] The adhesion strength and toughness of collagen / PVA hydrogel were tested. The specific implementation method is as follows:
[0051] The prepared hydrogel was adhered to different material surfaces and different joint surfaces of the human body, and the adhesion properties of the hydrogel were recorded with a digital camera. Figure 1 (a) The four materials are tightly bound to the hydrogel, indicating that the hydrogel has strong adhesion to different materials. Figure 1 (b) The hydrogel adhered to the back of the hand was lifted with tweezers, and the hydrogel remained in its original shape, indicating that the hydrogel has good toughness. Figure 1 (c) and 1(d) adhere the hydrogel to the wrist joint, bent finger joint, wrist joint, and elbow joint, showing that the composite hydrogel maintains good adhesion under different dynamic joints.
[0052] Example 5
[0053] This example was carried out using the product prepared in Example 1.
[0054] The collagen / PVA hydrogel wound dressing was subjected to tensile testing and its self-healing ability was tested as follows:
[0055] A circular hydrogel with a diameter of about 2.5 cm and a thickness of about 3 mm was stretched into a film, the thickness of which was negligible, and its length was measured with a ruler. Figure 2 As shown in (a), the size is more than 10 times that of the former. Figure 2 (b) shows that a hydrogel with a diameter of 3 cm was cut into two halves, one half was colored with rhodamine b, and the other half remained original. The cut ends were then joined together. After standing for a period of time, the hydrogel self-healed and could be stretched, indicating the good self-healing properties of the hydrogel.
[0056] Example 6
[0057] This example was carried out using the product prepared in Example 1.
[0058] The plasticity of collagen / PVA hydrogel was tested. The specific implementation method is as follows:
[0059] Place the same piece of dyed hydrogel into different molds, such as Figure 3 As shown, the hydrogel can be transformed into several different shapes, which demonstrates the good plasticity of the hydrogel and is beneficial for using the hydrogel in various applications.
[0060] Example 7
[0061] This example was carried out using the products prepared in Examples 1, 2, and 3.
[0062] like Figure 4 As shown, after the hydrogels of different components were co-cultured with Staphylococcus aureus (S. aureus) and Escherichia coli (E. coli) for 24 hours, obvious inhibition zones were observed around the hydrogels, indicating that the hydrogels had good antibacterial ability.
Claims
1. A collagen / PVA hydrogel wound dressing, characterized by: It uses collagen and PVA as the matrix, borax as the cross-linking agent, hydroxypropyl methylcellulose as the thickener, and polyhexamethylene biguanide as the antibacterial agent to form a hydrogel wound dressing by forming borate ester bonds.
2. A collagen / PVA hydrogel wound dressing according to claim 1, characterized in that: The mass percentage concentrations of collagen, PVA, borax, hydroxypropyl methylcellulose and polyhexamethylene biguanide are as follows: 0.5-3%, 2-10%, 2-6%, 1.5-2% and 0.05-0.15%.
3. The collagen / PVA hydrogel wound dressing according to claim 1, characterized in that: Borax is used as a cross-linking agent, and the concentration of borax is 2-6%.
4. A collagen / PVA hydrogel wound dressing according to claims 1-3, characterized in that: The collagen / PVA hydrogel wound dressing has cyclic plasticity, rapid self-healing, stretchability, antioxidant and antibacterial properties.
5. The collagen / PVA hydrogel wound dressing according to claims 1-4, characterized in that: The preparation method comprises the following steps: Step 1: Prepare a certain concentration of PBS solution with a pH of 7.4, a certain concentration of NaOH solution, and a 0.5 M glacial acetic acid solution. Step 2: Dissolve collagen in glacial acetic acid and adjust the pH to 7-7.4 with PBS and NaOH to obtain a 40% collagen stock solution. Then, weigh PVA and borax solids and dissolve them in water to prepare stock solutions with a concentration of 25%. Step 3: Prepare a polyhexamethylene biguanide stock solution with a concentration of 1%. Step 4: Add a certain amount of water to the PVA mother liquor and carboxymethyl propyl cellulose powder in a certain proportion and mix them evenly. After the two substances are completely mixed, stir them at 80°C for 15 minutes (heating in a water bath), cool the solution to room temperature, add a certain volume of collagen mother liquor and polyhexamethylene biguanide mother liquor and mix them evenly to form precursor solution I. Step 5: Use borax solution as precursor solution II. Step 6: The precursor solution I and the precursor solution II described in step 4 and step 5 are uniformly mixed in a certain volume ratio using a vortex mixer to form a hydrogel wound dressing, wherein the mass percentages of collagen, PVA, borax, hydroxymethylpropyl cellulose, and polyhexamethylene biguanide are 0.5-3%, 2-10%, 2-6%, 1.5-2%, and 0.05-0.15%, respectively.
6. Use of the collagen / PVA hydrogel wound dressing according to claims 1-7 as a hydrogel membrane in the field of healing infectious irregular wounds and joint wounds.