Preparation method of hemostatic hydrogel and product thereof
By combining chitosan, mesoporous silica, and photocurable hydrogel, a hemostatic hydrogel was prepared, which solved the problems of adhesion and strength of hemostatic materials in deep bleeding wounds, and achieved rapid hemostasis and high strength.
Patent Information
- Application Number
- CN202511944138.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-22
- Publication Date
- 2026-03-20
AI Technical Summary
Existing hemostatic materials have problems such as poor adhesion, slow hemostasis, easy adhesion causing secondary damage, and lack of bioactivity when dealing with deep, irregular or pulsating bleeding wounds. In addition, chitosan hydrogel has poor stability and insufficient mechanical strength in humid environments.
Chitosan was combined with mesoporous silica and photocurable hydrogel. The mesoporous silica absorbed water, causing the blood clotting components to shrink rapidly, thus preparing a hemostatic hydrogel. The hemostatic gel was then formed using photocuring technology.
It achieves a balance between hemostasis speed and gel strength, exhibiting excellent hemostatic properties and mechanical strength, and the preparation method is simple and easy to operate.
Abstract
Description
Technical Field
[0001] This invention relates to a method for preparing a hemostatic hydrogel and its product, specifically a hemostatic hydrogel synthesized primarily from chitosan (CS), mesoporous silica (M), and photocurable hydrogel. This invention belongs to the field of nanobiomedical materials. Background Technology
[0002] In clinical medicine, trauma emergency care, and military medicine, rapid, efficient, and safe hemostasis techniques are crucial for reducing the risk of blood loss and saving lives. Traditional hemostatic materials such as gauze and gelatin sponges, while widely used, often have limitations when dealing with deep, irregular, or pulsating wounds, including poor adhesion, slow hemostasis, easy adhesion leading to secondary damage, and lack of bioactivity.
[0003] In recent years, hemostatic materials based on natural biological polysaccharides have attracted widespread attention due to their good biocompatibility, biodegradability, and inherent bioactivity. Among them, chitosan, as a cationic polysaccharide, can effectively adsorb negatively charged blood cells and platelets through electrostatic interactions after the amino groups on its molecular chain are protonated, thereby activating the coagulation cascade reaction. It also has the unique advantages of broad-spectrum antibacterial activity and tissue repair promotion, and is considered an ideal matrix for hemostatic materials.
[0004] However, pure chitosan materials still suffer from insufficient mechanical strength, poor stability in humid environments, and weak tissue adhesion in their application forms (such as powders and films). To address these challenges, combining chitosan with hydrogel technology has become an important research direction. Hydrogels can mimic the hydrophilic three-dimensional network structure of the extracellular matrix, providing a moist healing microenvironment for wounds, and significantly improving the mechanical properties, morphological adaptability, and controllable degradation of materials through physical or chemical cross-linking.
[0005] Despite the great potential of chitosan hydrogels in the field of hemostasis, existing technologies still face many bottlenecks: in particular, it is difficult to balance hemostasis speed and gel strength, rapid gelation often sacrifices strength, while high-strength gels may gel slowly. Summary of the Invention
[0006] To address the difficulty in balancing hemostasis speed and gel strength in existing technologies, where rapid gel formation often sacrifices strength and high-strength gels may suffer from slow gel formation, this invention aims to provide a method for preparing a hemostatic hydrogel. Based on photocurable chitosan loaded with mesoporous silica, the method utilizes the excellent adsorption capacity of mesoporous silica to absorb a large amount of water, causing the coagulation components in the blood to contract rapidly and thus achieve hemostasis.
[0007] Another object of the present invention is to provide a hemostatic hydrogel product prepared by the above method.
[0008] The objective of this invention is achieved through the following method: a method for preparing a hemostatic hydrogel, which uses chitosan (CS), mesoporous silica (M), and photocurable hydrogel as main raw materials to synthesize the hemostatic hydrogel, comprising the following steps: (1) Disperse 0.5~2g of CS into 50 ml of 0.1M hydrochloric acid solution, stir magnetically overnight at room temperature to ensure that CS is completely dissolved, and store the solution at 4℃; (2) Disperse 50~200mg MSNs in a prepared 40%~60% β-GP solution. After it is completely dissolved, slowly add the prepared CS solution. Stir the mixture magnetically until it is homogeneous.
[0009] (3) The above solution was mixed thoroughly with 20-30 wt% N-acryloylglycine amide (NAGA) and 0.1 wt% photoinitiator (Irgacure 2959). The solution was then injected into the mold and subjected to 365nm UV (10 mW / cm²). 2 After irradiation with a light source for 5-10 minutes, a hemostatic gel can be formed.
[0010] The degree of deacetylation of the CS is 80%~95%.
[0011] The CS mass-to-volume ratio is 0.3-2.5%.
[0012] The concentration ratio of CS to β-GP is 1:15 to 1:7.5.
[0013] MSNs have sizes ranging from 100 to 400 nm and specific surface areas ranging from 150 to 200 m². 2 / g.
[0014] This invention provides a hemostatic hydrogel, prepared according to any of the methods described above.
[0015] Hemostatic performance: The hemostatic performance of the material was evaluated using the blood coagulation index (BCI). The specific experimental procedures are as follows: Take approximately 0.5 cm x 0.5 cm of the prepared hydrogel pieces and place them in 50 ml centrifuge tubes, incubating at 37°C for 5 min. Add 250 μl of fresh rat blood to a preheated centrifuge tube, then add 25 μl of 0.2 M CaCl2 solution, and incubate at 37°C for 3 min. Remove the centrifuge tube, add 25 ml of deionized water, and incubate again at 37°C for 3 min. Remove the supernatant from the centrifuge tube with a pipette, and measure the absorbance at 545 nm using an ELISA reader, denoted as ODP. Use an empty centrifuge tube to measure its absorbance at 545 nm as a negative control, denoted as ODo. Simultaneously, use a centrifuge tube with the same volume of blood added to it and incubated with deionized water for 5 min as the experimental group, and measure its absorbance at 545 nm as a positive control, denoted as Odt. The coagulation index (%) is calculated as ODP - ODo / Odt - ODo x 100%. Table 2 shows the hemostatic index of the prepared hydrogel and other hemostatic materials. As shown in Table 2, the coagulation index of the prepared hemostatic hydrogel was 15.6%, while the coagulation indices of the bandage and gauze were 60.8% and 63.2%, respectively, indicating that the prepared hemostatic hydrogel has excellent hemostatic properties.
[0016] The advantages of this invention are: (1) The hemostatic hydrogel of the present invention has good swelling ability and hemostatic ability of hydrogel. At the same time, the addition of mesoporous material enhances the rigidity of hydrogel, so that the hemostatic speed and gel strength are balanced.
[0017] (2) The preparation method in this invention is simple and easy to operate, and can further meet the needs of production and application. Detailed Implementation
[0018] The technical solution of the present invention will be further described below through specific embodiments. These embodiments are further illustrations of the present invention and do not limit the scope of the invention.
[0019] Example 1 A method for preparing a hemostatic hydrogel, characterized in that the hemostatic hydrogel is synthesized using chitosan (CS), mesoporous silica (M), and photocurable hydrogel as main raw materials, comprising the following steps: (1) Disperse 1g of CS into 50 ml of 0.1M hydrochloric acid solution, stir magnetically overnight at room temperature to ensure that CS is completely dissolved, and store the solution at 4℃; (2) 150 mg MSNs were dispersed in a prepared 55% β-GP solution. After the solution was completely dissolved, the prepared CS solution was slowly added dropwise. The mixture was then magnetically stirred until homogeneous. (3) The above solution is mixed with 25 wt% N-acryloylglycine amide NAGA and 0.1 wt% Irgacure 2959. The solution is injected into a mold and irradiated with a 365nm UV (10 mW / cm2) light source for 10 min to form a hemostatic gel.
[0020] The MSNs used in this embodiment have a size of 200 nm, and their specific surface area, as measured by BST, is 176.26 m². 2 / g, and BJH measured its pore size to be 14.23 nm.
[0021] Table 1 shows the tensile properties of the hemostatic hydrogel prepared in this embodiment. The prepared hydrogel has a tensile strength of 0.15 MPa, an elongation at break of 17%, and a Young's modulus of 0.24 MPa. From Table 1: .
[0022] Example 2 Hemostatic performance: The hemostatic performance of the material was evaluated using the blood coagulation index (BCI). The specific experimental procedures are as follows: Take approximately 0.5 cm x 0.5 cm of the prepared hydrogel pieces and place them in 50 ml centrifuge tubes, incubating at 37°C for 5 min. Add 250 μl of fresh rat blood to a preheated centrifuge tube, then add 25 μl of 0.2 M CaCl2 solution, and incubate at 37°C for 3 min. Remove the centrifuge tube, add 25 ml of deionized water, and incubate again at 37°C for 3 min. Remove the supernatant from the centrifuge tube with a pipette, and measure the absorbance at 545 nm using an ELISA reader, denoted as ODP. Use an empty centrifuge tube to measure its absorbance at 545 nm as a negative control, denoted as ODo. Simultaneously, use a centrifuge tube with the same volume of blood added to it and incubated with deionized water for 5 min as the experimental group, and measure its absorbance at 545 nm as a positive control, denoted as Odt. The coagulation index (%) is calculated as ODP - ODo / Odt - ODo x 100%. Table 2 shows the hemostatic index of the prepared hydrogel and other hemostatic materials. Table 2 shows that the coagulation index of the prepared hemostatic hydrogel was 15.6%, while the coagulation indices of the bandage and gauze were 60.8% and 63.2%, respectively, indicating that the prepared hemostatic hydrogel has excellent hemostatic properties. .
Claims
1. A method for preparing a hemostatic hydrogel, characterized in that, A hemostatic hydrogel synthesized primarily from chitosan (CS), mesoporous silica (M), and photocurable hydrogel includes the following steps: (1) Disperse 0.5~2g of CS into 50 ml of 0.1M hydrochloric acid solution, stir magnetically overnight at room temperature to ensure that CS is completely dissolved, and store the solution at 4℃; (2) Disperse 50~200mg MSNs in a prepared 40%~60% β-GP solution. After it is completely dissolved, slowly add the prepared CS solution. Stir the mixture magnetically until it is homogeneous. (3) The above solution is mixed with 20~30 wt% N-acrylyl glycine amide NAGA and 0.1 wt% photoinitiator (Irgacure2959) until homogeneous. The solution is then injected into a mold and irradiated with a 365nm UV (10 mW / cm2) light source for 5~10 min to form a hemostatic gel.
2. The method for preparing a hemostatic hydrogel according to claim 1, characterized in that, The degree of deacetylation of the CS is 80%~95%.
3. The method for preparing a hemostatic hydrogel according to claim 1, characterized in that, The concentration ratio of CS to β-GP is 1:15 to 1:7.
5.
4. The method for preparing a hemostatic hydrogel according to claim 1, characterized in that... The MSNs have a size of 100-400 nm and a specific surface area of 150-200 m². 2 / g.
5. A method for preparing a hemostatic hydrogel, characterized in that... Prepared according to any one of claims 1-4.