3D structure endotoxin adsorption material and preparation method and application thereof

Abstract

The invention discloses an endotoxin adsorption material with a 3D structure and a preparation method and application thereof, and relates to the technical field of biomedical materials.The preparation method comprises the steps that polyacrylonitrile, polyethyleneimine and a mixed solvent serve as raw materials to prepare a spinning solution, and the mass ratio of polyacrylonitrile to polyethyleneimine is (0.5-4): 1; installing an electrostatic spinning device, horizontally arranging a conductive metal plate collector between a spinning nozzle and a grounding metal plate which are opposite to each other, installing a high-pressure gas ejector above the collector, injecting the obtained spinning solution into the spinning nozzle, applying voltage, enabling the spinning solution and the collector to have the same charge, and performing a spinning process; a 3D nanofiber aggregate is obtained on a collector; and carrying out high-temperature crosslinking treatment on the obtained 3D nanofiber aggregate to obtain the endotoxin adsorption material with the 3D structure. The obtained adsorption material has the stability of a 3D structure and has good endotoxin blood perfusion adsorption performance.

Description

Technical Field

[0001] The present invention relates to the technical field of biomedical materials, and in particular to a 3D-structured endotoxin adsorption material and a preparation method and application thereof. Background Art

[0002] Sepsis is a fatal organ dysfunction syndrome caused by a dysregulated host response to infection, and traditional treatments are limited. Endotoxin (LPS) released by Gram-negative bacteria is a core pathological factor. By binding to CD14 / TLR4 receptors on monocytes and macrophages, it activates a cascade of inflammatory mediators, including TNF-α and IL-1, resulting in an "immune inflammatory storm." Even trace amounts of LPS (pg / mL) can synergize complement activation and coagulation disorders through LBP-mediated sensitization, leading to microcirculatory impairment and disseminated intravascular coagulation, ultimately triggering a cascade of multi-organ failure.

[0003] Hemoperfusion technology has attracted considerable attention due to its ability to remove pathogenic substances through specific or nonspecific adsorption. The core of this technology's efficacy lies in the performance characteristics of the adsorption material. Compared to traditional materials, organic polymer materials have become the mainstream research direction due to their advantages such as adjustable molecular structure, easy surface functionalization, and good biocompatibility. This type of material mainly presents two structural forms: one is granular resin materials, which have complex and uneven flow channel structures and are prone to inducing coagulation; the other is hollow fiber membrane materials, which, although having a relatively uniform pore structure, face challenges such as difficulty in modification and limited effective adsorption area.

[0004] The emergence of novel nanofiber materials has provided new insights into the development of hemoperfusion adsorbents. For example, patent publication CN112871139A discloses a whole blood perfusion adsorbent that innovatively combines natural polymer nanofibers with inorganic or organic functional fillers to create microspheres with a large, porous nanofiber network structure.

[0005] At present, electrospinning technology has developed to maturity, and large-scale industrial equipment can achieve large-scale production of nanofiber materials. Therefore, electrospun nanofibers are expected to become an ideal choice for endotoxin adsorbents. However, the materials prepared by traditional electrospinning technology are usually two-dimensional film structures, which are difficult to directly use as filling materials for blood perfusion adsorbents. For example, patent document No. CN114669282A discloses an endotoxin adsorbent and its preparation method. This method uses electrospinning to prepare a two-dimensional polymer-based nanofiber membrane, which still needs to be modified.

[0006] The production of electrospun materials with three-dimensional structures typically requires auxiliary processes such as freeze-drying, which are complex and energy-intensive. For example, patent publication CN108404823A describes an invention that first disperses an electrospun nanofiber membrane in an aqueous solution, then freeze-drying and thermally crosslinking the membrane to produce a three-dimensional nanofiber aerogel.

[0007] In summary, 3D nanofibers, with their high surface area and high fillability, are an ideal choice for preparing endotoxin adsorbents. However, this field still faces two challenges: first, optimizing efficient methods for constructing 3D structures, and second, further improving endotoxin adsorption performance. Breakthroughs in these technical challenges will help advance the clinical application of a new generation of hemoperfusion adsorbents. Summary of the Invention

[0008] To further improve the efficiency of 3D structure construction and enhance endotoxin adsorption performance, the present invention provides a method for preparing a 3D endotoxin adsorbent material using airflow and charge-assisted electrospinning technology. This method is simple to operate and can produce materials with varying densities and porosities to meet the differentiated needs of different application scenarios. The resulting adsorbent material exhibits 3D structural stability, a high specific surface area, and uniformly distributed adsorption sites, significantly improving endotoxin adsorption performance during hemoperfusion.

[0009] The specific technical solutions adopted are as follows: A method for preparing a 3D structured endotoxin adsorption material, comprising: (1) preparing a spinning solution using polyacrylonitrile, polyethyleneimine and a mixed solvent as raw materials, wherein the mass ratio of polyacrylonitrile to polyethyleneimine is 0.5-4:1; (2) Installing an electrospinning device, placing a conductive metal plate collector horizontally between the opposite spinning nozzles and the grounded metal plate, installing a high-pressure gas jet above the collector, injecting the resulting spinning solution into the spinning nozzle, applying voltage so that the spinning solution and the collector have the same charge and performing the spinning process, and obtaining a 3D nanofiber aggregate on the collector; (3) The obtained 3D nanofiber aggregate is subjected to high-temperature cross-linking treatment to obtain the 3D structured endotoxin adsorption material.

[0010] The present invention utilizes a high-voltage electric field to form a jet of spinning liquid, which then flows from the spinning nozzle toward a grounded metal plate. Simultaneously, a vertically downward high-pressure airflow is applied above a conductive metal plate collector, guiding the spinning liquid downward and assisting its collection by the conductive metal plate collector below. Furthermore, the conductive metal plate collector and the spinning liquid are charged with the same polarity. The electrostatic repulsion generated by these charges effectively inhibits the dense accumulation of fibers and encourages their spatial dispersion across the collector surface. The synergistic effects of electrostatic repulsion and high-pressure airflow guide the fibers in situ on the collector, forming a fluffy, three-dimensional mesh structure.

[0011] Unlike the traditional method of collecting two-dimensional materials on a grounded metal plate, this method maintains the same polarity charge by applying an external electric field on the conductive metal plate collector. Combined with the regulation of airflow intensity, it achieves the directional deposition of fibers on the conductive metal plate collector and the precise regulation of the material porosity. Finally, a three-dimensional nanofiber aggregate with a highly connected open pore network is obtained, which can be used as an efficient endotoxin adsorption material.

[0012] Preferably, in step (1), the number average molecular weight of polyacrylonitrile is 50,000-250,000, and the number average molecular weight of polyethyleneimine is 800-10,000.

[0013] Preferably, in the spinning solution, the mass concentration of polyacrylonitrile is 5-25 wt%, and the mixed solvent is two or more of N,N-dimethylformamide, acetone, N,N-dimethylacetamide, dimethyl sulfoxide, and water.

[0014] Preferably, the mixing process of the solute and the solvent in step (1) is as follows: placing the mixed solvent in a constant temperature water bath, adding polyacrylonitrile thereto and stirring, then adding polyethyleneimine, and performing constant temperature magnetic stirring to obtain the spinning solution.

[0015] Preferably, the stirring time in step (1) is 12-24 h, and the stirring temperature is 30-45°C.

[0016] Preferably, in step (2), the inner diameter of the spinning nozzle is 0.2-0.5 mm, the voltage applied to the spinning solution is 8-20 kV, the spinning speed is 0.5-2 mL / h, and the spinning time is 5-10 h.

[0017] Preferably, in step (2), the conductive metal plate collector is a copper plate or an iron plate, the plate size is a square with a side length of 15 cm, with insulating foot stickers attached to the four corners and metal aluminum foil adhered to the surface, and the voltage applied to the conductive metal plate collector is 0.2~5kV.

[0018] Preferably, in step (2), the length of the high-pressure gas injector is 10-25 cm, the slit width of the gas outlet of the high-pressure gas injector is 0.1-1 cm, the high-pressure gas injector is located 15-30 cm above the conductive metal plate receiver, the distance from the spinning nozzle to the conductive metal plate is 5-10 cm, and the distance to the grounded metal plate is 15-20 cm.

[0019] Preferably, the gas ejected from the high-pressure gas ejector in step (2) is air, nitrogen or argon. If the high-pressure gas ejection is controlled by flow rate, the gas flow rate is 5 to 30 cm / s; if the high-pressure gas ejection is controlled by pressure, the gas pressure is 2 to 10 MPa. By controlling the gas flow rate or pressure, the density and porosity of the obtained product can be controlled.

[0020] Preferably, the spinning conditions in step (2) are: ambient humidity of 40-85% and ambient temperature of 21-29°C.

[0021] Preferably, the conditions for high-temperature cross-linking treatment in step (3) are: vacuum degree -0.09 to -0.1 MPa, temperature 150 to 180°C, and time 6 to 12 h.

[0022] During the high-temperature cross-linking process, residual solvent is removed. Simultaneously, the acetoxy groups on the polyacrylonitrile molecular chains cross-link with the amino groups on the polyethyleneimine, forming a stable three-dimensional network structure. This prevents fiber shedding or structural collapse during subsequent use. Furthermore, the abundant positively charged tertiary amino groups on the polyethyleneimine can bind to negatively charged endotoxin molecules through electrostatic attraction.

[0023] The present invention also provides a 3D structured endotoxin adsorption material, which is prepared by the preparation method of the 3D structured endotoxin adsorption material.

[0024] The 3D structured endotoxin adsorption material prepared according to the above method has a unique three-dimensional nanofiber network structure, a high specific surface area and through-pores.

[0025] Furthermore, the present invention also applies the 3D structured endotoxin adsorption material to the preparation of sepsis treatment products.

[0026] The prepared 3D structured endotoxin adsorption material is used to prepare sepsis treatment products, which can achieve efficient removal of LPS while ensuring the low flow resistance characteristics of whole blood perfusion. It is suitable for early intervention of sepsis and prevention and treatment of postoperative endotoxemia.

[0027] Compared with the prior art, the present invention has the following beneficial effects: (1) The present invention adopts a high-pressure airflow blowing molding method, which is relatively simple to operate and can obtain 3D structured endotoxin adsorption materials with different densities and porosities by controlling experimental conditions.

[0028] (2) Compared with conventional endotoxin adsorption materials, the polyethyleneimine in the 3D structured endotoxin adsorption material provided by the present invention has better dispersibility, which ensures the uniform distribution of endotoxin adsorption sites on the fiber. At the same time, the contact points between the nanofiber monofilaments are thermally cross-linked to form a structure similar to "welding", which ensures the mechanical stability of the nanofiber 3D structure.

[0029] (3) Compared with the disclosed patents for endotoxin nanofiber adsorption materials, the material of the present invention can provide a higher specific surface area, thus having a higher endotoxin adsorption capacity, while ensuring a lower blood protein adsorption capacity and high blood compatibility, and cells will basically not block the pores, resulting in a better blood perfusion treatment effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 Diagram of the preparation device for 3D structured endotoxin adsorption materials.

[0031] Figure 2 These are SEM images of the 3D structured endotoxin adsorption materials in the examples and comparative examples. Specific implementation methods The present invention will be further described below with reference to the accompanying drawings and examples. It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention.

[0032] Example 1 S01. Add 7.5 g of vacuum-dried polyacrylonitrile (MW 250,000) to 85 mL of a 1:1 volume ratio of N,N-dimethylformamide (DMF) and acetone mixture in a 30°C water bath. Stir for 1 h, then add 2.5 g of polyethyleneimine (MW 1600). Stir in a 40°C water bath for 12 h to obtain a spinning solution.

[0033] S02. Press Figure 1 As shown, an electrospinning device is installed, and a 15 cm × 15 cm conductive metal plate collector made of copper plate is placed horizontally between the relative spinning nozzle and the grounded metal plate. A high-pressure gas ejector is placed 25 cm above the conductive metal plate collector. The length of the ejector is 25 cm, and the slit width of the ejector outlet is 0.3 mm. The ejected gas is nitrogen, and the gas flow rate is 30 cm / s.

[0034] S03. The spinning solution from step S01 was placed in a spinning nozzle for electrospinning. After spinning for 10 hours, a 3D nanofiber material was obtained. The electrospinning process parameters during the process were: a spinning nozzle inner diameter of 0.41 mm, a voltage of 15 kV applied to the spinning solution, a voltage of 2 kV applied to the conductive metal plate collector, both the spinning solution and the collector were positively charged, a spinning solution flow rate of 1 mL / h, an ambient humidity of 75%, and an ambient temperature of 25°C. S04. The 3D nanofiber material obtained in step S03 is transferred to a vacuum oven for high-temperature crosslinking. The vacuum degree of the vacuum oven is -0.1 MPa, the temperature is 150°C, and the crosslinking time is 6 h to obtain a 3D structured endotoxin adsorption material.

[0035] Example 2 S11. After vacuum drying, 8 g of polyacrylonitrile (molecular weight, 100,000) was added to 85 mL of a mixed solvent of N,N-dimethylformamide (DMF), acetone, and water (volume ratio of 7:2.5:0.5). The mixture was heated in a 45°C water bath and stirred for 1 hour. After that, 2 g of polyethyleneimine (molecular weight, 1600) was added and stirred in a 40°C water bath for 12 hours to obtain a spinning solution.

[0036] S12. Press Figure 1 As shown, an electrospinning device is installed, and a 15 cm × 15 cm conductive metal plate collector made of copper plate is placed horizontally between the relative spinning nozzle and the grounded metal plate. A high-pressure gas ejector is placed 25 cm above the conductive metal plate collector. The length of the ejector is 25 cm, the slit width of the ejector outlet is 0.3 mm, the ejected gas is nitrogen, and the gas flow rate is 15 cm / s.

[0037] S13. The spinning solution from step S11 was placed in a spinning nozzle for electrospinning. After spinning for 10 h, a 3D nanofiber material was obtained. During the electrospinning process, the following parameters were used: an inner diameter of the spinning nozzle of 0.41 mm, a voltage of 15 kV applied to the spinning solution, a voltage of 1 kV applied to the conductive metal plate collector, both the spinning solution and the collector were positively charged, a spinning solution flow rate of 1 mL / h, an ambient humidity of 75%, and an ambient temperature of 25°C.

[0038] S14. The 3D nanofiber material obtained in step S13 was transferred to a vacuum oven for high-temperature crosslinking. The vacuum degree of the vacuum oven was -0.1 MPa, the temperature was 170°C, and the crosslinking time was 8 h to obtain a 3D structured endotoxin adsorption material.

[0039] Example 3 S21. Add 7.5 g of vacuum-dried polyacrylonitrile (MW 250,000) to 85 mL of a mixed solvent of N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), and water (volume ratio of 7:2:1). Heat in a 40°C water bath and stir for 1 h. Then, add 2.5 g of polyethyleneimine (MW 1600) and stir in a 40°C water bath for 12 h to obtain a spinning solution.

[0040] S22. Press Figure 1 As shown, an electrospinning device is installed, and a 15 cm × 15 cm conductive metal plate collector made of copper plate is placed horizontally between the relative spinning nozzle and the grounded metal plate. A high-pressure gas ejector is placed 25 cm above the conductive metal plate collector. The length of the ejector is 25 cm, the slit width of the ejector outlet is 0.3 mm, the ejected gas is nitrogen, and the gas flow rate is 10 cm / s.

[0041] S23. The spinning solution from step S21 was placed in a spinning nozzle for electrospinning. After spinning for 10 h, a 3D nanofiber material was obtained. During the electrospinning process, the parameters were as follows: the nozzle was 0.41 mm thick, a voltage of 15 kV was applied to the spinning solution, a voltage of 5 kV was applied to the conductive metal plate collector, both the spinning solution and the collector were positively charged, the spinning solution flow rate was 0.8 mL / h, the ambient humidity was 75%, and the ambient temperature was 25°C.

[0042] S24. The 3D nanofiber material obtained in step S23 is transferred to a vacuum oven for high-temperature crosslinking. The vacuum degree of the vacuum oven is -0.1 MPa, the temperature is 180°C, and the crosslinking time is 12 h to obtain a 3D structured endotoxin adsorption material.

[0043] Example 4 S31. Add 7.5 g of vacuum-dried polyacrylonitrile (MW 100,000) to 85 mL of a mixed solvent of N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), and water (volume ratio of 7:2:1). Heat in a 40°C water bath and stir for 1 h. Then, add 2.5 g of polyethyleneimine (MW 1600) and stir in a 40°C water bath for 12 h to obtain a spinning solution.

[0044] S32. Press Figure 1 As shown, an electrospinning device is installed, and a 15 cm × 15 cm conductive metal plate collector made of copper plate is placed horizontally between the relative spinning nozzle and the grounded metal plate. A high-pressure gas ejector is placed 25 cm above the conductive metal plate collector. The length of the ejector is 25 cm, and the slit width of the ejector outlet is 0.3 mm. The ejected gas is nitrogen, and the gas flow rate is 25 cm / s.

[0045] S33. The spinning solution from step S31 was placed in a spinning nozzle for electrospinning. After spinning for 10 hours, a 3D nanofiber material was obtained. The electrospinning process parameters during the process were: a spinning nozzle inner diameter of 0.41 mm, a voltage of 15 kV applied to the spinning solution, a voltage of 5 kV applied to the conductive metal plate collector, both the spinning solution and the collector were positively charged, a spinning solution flow rate of 1 mL / h, an ambient humidity of 75%, and an ambient temperature of 25°C. S34. The 3D nanofiber material obtained in step S33 was transferred to a vacuum oven for high-temperature crosslinking. The vacuum degree of the vacuum oven was -0.1 MPa, the temperature was 175°C, and the crosslinking time was 12 h to obtain a 3D structured endotoxin adsorption material.

[0046] Comparative Example 1 The difference between this comparative example and Example 1 is that a traditional roller is used to collect the nanofibers, the spinning device is not provided with a conductive metal plate collector and a high-pressure gas injector, and no positive voltage is applied to the conductive metal plate collector.

[0047] Comparative Example 2 The difference between this comparative example and Example 4 is that no polyethyleneimine is added and no thermal cross-linking method is used for post-treatment.

[0048] Test methods and performance (1) Morphology analysis In Examples 1-4, the SEM images of the 3D structured endotoxin adsorbent materials are as follows: Figure 2 As shown in the figure, the 3D structured endotoxin adsorption material prepared by airflow and charge assistance has a fluffy structure inside. The addition of dimethyl sulfoxide solvent makes the classic spinning material different inside, with different internal structures. The cross-linking points are generated between the fibers through thermal cross-linking, thereby improving the mechanical strength of the material. Figure 2 Compared with the 2D structure endotoxin adsorbent material collected by the traditional drum in Comparative Example 1, the 3D structure endotoxin adsorbent material in the embodiment has obvious gaps inside, which makes it have a good specific surface area. Figure 2 For comparison, the 3D structured endotoxin adsorption material of Comparative Example 2, which does not add PEI and is not thermally cross-linked, has a material with too loose internal fibers and low mechanical strength.

[0049] (2) Dynamic adsorption effect of endotoxin adsorption materials on endotoxins in different systems A certain amount of endotoxin working standard was dissolved in Tris-HCl buffer and heparin sodium anticoagulated rabbit whole blood to prepare endotoxin buffer solution with an endotoxin concentration of 5 EU / mL and endotoxin-containing rabbit whole blood, respectively.

[0050] The 3D structured endotoxin adsorption material prepared in Example 1 was used as the experimental group, and the endotoxin adsorption materials prepared in Comparative Examples 1 and 2 were used as the control group. The samples of the experimental group and the control group were placed in a replaceable filter head. The adsorption rates of the experimental group and the control group samples on endotoxins in different systems were tested through continuous adsorption experiments. The experimental results are shown in Table 1. The results indicate that, in a buffer solution, the 3D-structured endotoxin adsorbent prepared in Example 1 can maintain an adsorption rate of approximately 80% for endotoxin in rabbit whole blood (within 3 hours), while the 2D-structured endotoxin adsorbent received by a conventional drum can only remove 54% of endotoxin within 3 hours. The 3D-structured endotoxin adsorbent without PEI in Comparative Example 2 cannot effectively adsorb endotoxin in the blood.

[0051] Table 1 Endotoxin adsorption performance of different samples (3) Adsorption effect of endotoxin adsorption materials on total protein, albumin and fibrinogen in rabbit plasma The endotoxin adsorption materials in the embodiment and the comparative example were taken respectively, with a volume of 0.5 cm × 0.5 cm × 0.5 cm, placed in a centrifuge tube, 50 mL of anticoagulant rabbit plasma was added, and the tube was placed in a constant temperature shaking incubator for shaking adsorption. After the adsorption was completed, samples were taken, and the concentrations of total plasma protein, albumin, and fibrinogen before and after adsorption were detected using a fully automatic biochemical analyzer and a coagulometer, and the adsorption rates of the samples for total plasma protein, albumin, and fibrinogen were calculated.

[0052] The experimental results are shown in Table 2. Compared with Comparative Examples 1 and 2, the 3D structured endotoxin adsorption material prepared in Example 1 has less nonspecific adsorption of proteins in the blood and has higher blood compatibility.

[0053] Table 2 Protein adsorption rate of different samples (4) Hemolytic properties of endotoxin adsorption materials Add 8 mL of heparin sodium anticoagulated rabbit whole blood and 10 mL of 0.9% normal saline into a centrifuge tube and mix well to obtain rabbit blood dilution solution.

[0054] Take five centrifuge tubes and number them 1 to 5. Add 0.2 mL of rabbit blood dilution and 10 mL of 0.9% normal saline to centrifuge tube 1 as a negative control; add 0.2 mL of rabbit blood dilution and 10 mL of deionized water to centrifuge tube 2 as a positive control; add 0.2 mL of rabbit blood dilution and 10 mL of 0.9% normal saline to centrifuge tubes 3 to 5, respectively. Then, add the endotoxin adsorbent materials of Example 3, Comparative Example 1, and Comparative Example 2 to the corresponding centrifuge tubes, respectively. Place the five centrifuge tubes in a constant temperature shaking incubator for shaking and centrifugation. After the supernatant is collected, the absorbance is measured and the hemolysis rate of each sample is calculated.

[0055] The hemolysis rate H is defined as: in, A s is the absorbance of the sample; A n is the absorbance of the negative control group; A p is the absorbance of the positive control group.

[0056] Table 3 Hemolytic properties of different samples As can be seen from Table 3, all three samples meet the national standard requirement for biomaterials, which requires a hemolysis rate of less than 5%, but the 3D structured endotoxin adsorption material prepared in Example 3 has the lowest hemolysis rate, proving that it has the best blood compatibility.

[0057] In summary, the 3D-structured endotoxin adsorption material prepared in the present invention has a good specific adsorption effect on endotoxins, and the adsorption rate can be maintained at more than 80% within 3 hours. It can effectively remove endotoxins from plasma and can meet the basic clinical needs for hemoperfusion treatment of sepsis. It also has good blood compatibility and high anti-protein viscosity, and is particularly suitable for blood purification treatment of sepsis patients.

[0058] The embodiments described above provide a detailed description of the technical solutions of the present invention. It should be understood that the above are only specific embodiments of the present invention and are not intended to limit the present invention. Any modifications, supplements or similar substitutions made within the scope of the principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A method for preparing a 3D structured endotoxin adsorption material, characterized in that: include: (1) preparing a spinning solution using polyacrylonitrile, polyethyleneimine and a mixed solvent as raw materials, wherein the mass ratio of polyacrylonitrile to polyethyleneimine is 0.5-4:1; (2) Installing an electrospinning device, placing a conductive metal plate collector horizontally between the opposite spinning nozzles and the grounded metal plate, installing a high-pressure gas jet above the collector, injecting the resulting spinning solution into the spinning nozzle, applying voltage so that the spinning solution and the collector have the same charge and performing the spinning process, and obtaining a 3D nanofiber aggregate on the collector; (3) The obtained 3D nanofiber aggregate is subjected to high-temperature cross-linking treatment to obtain the 3D structured endotoxin adsorption material.

2. The method for preparing the 3D structured endotoxin adsorbent material according to claim 1, characterized in that: The number average molecular weight of the polyacrylonitrile described in step (1) is 50,000-250,000, and the number average molecular weight of the polyethyleneimine is 800-10,000.

3. The method for preparing the 3D structured endotoxin adsorbent material according to claim 1, wherein: In the spinning solution, the mass concentration of the polyacrylonitrile is 5-25 wt%, and the mixed solvent is two or more of N,N-dimethylformamide, acetone, N,N-dimethylacetamide, dimethyl sulfoxide, and water.

4. The method for preparing the 3D structured endotoxin adsorbent material according to claim 1, wherein: In step (2), the inner diameter of the spinning nozzle is 0.2-0.5 mm, the voltage applied to the spinning solution is 8-20 kV, the spinning speed is 0.5-2 mL / h, and the spinning time is 5-10 h.

5. The method for preparing the 3D structured endotoxin adsorbent material according to claim 1, wherein: The voltage applied to the conductive metal plate collector in step (2) is 0.2~5 kV.

6. The method for preparing a 3D structured endotoxin adsorbent material according to claim 1, wherein: The high-pressure gas injector described in step (2) is located 15 to 30 cm above the conductive metal plate collector; In step (2), the gas ejected by the high-pressure gas ejector is air, nitrogen or argon. If the high-pressure gas ejection is controlled by flow rate, the gas flow rate is 5 to 30 cm / s. If the high-pressure gas ejection is controlled by pressure, the gas pressure is 2 to 10 MPa.

7. The method for preparing a 3D structured endotoxin adsorbent material according to claim 1, wherein: The spinning conditions in step (2) are: ambient humidity of 40-85% and ambient temperature of 21-29°C.

8. The method for preparing a 3D structured endotoxin adsorbent material according to claim 1, wherein: The conditions for high-temperature cross-linking treatment in step (3) are: vacuum degree -0.09~-0.1 MPa, temperature 150~180°C, and time 6~12 h.

9. A 3D structured endotoxin adsorption material, characterized in that: The 3D structured endotoxin adsorption material is prepared by the preparation method of any one of claims 1-8.

10. Use of the 3D structured endotoxin adsorption material according to claim 9 in preparing a sepsis treatment product.

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