CN110841602B - Blood purification material based on mussel bionic chemistry and preparation method thereof - Google Patents
Blood purification material based on mussel bionic chemistry and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a blood purification material based on mussel bionic chemistry and a preparation method thereof, wherein the blood purification material sequentially comprises a porous adsorption base material, an adsorption layer and a coating film from inside to outside, the adsorption layer is one or more of polymyxin B sulfate, polylysine hydrochloride, polyethyleneimine or polydopamine, and is wound on the porous adsorption base material in a molecular chain form; the coating film is a polyvinyl butyral-gallic acid film or a polyvinyl butyral film. The blood purification material is designed based on mussel bionic chemistry, has the advantages of simplicity, convenience, mild condition, environmental friendliness and no influence on the material body basically, and is applied to the field of blood purification medical appliances.
Description
Technical Field
The invention belongs to the field of biochemical separation and biomedical materials, and particularly relates to a blood purification material based on mussel bionic chemistry and a preparation method thereof.
Background
In the existing preparation process of the medical instrument material for purifying blood, the adsorbent is often required to be modified, and the coating material is usually PVB, collodion and the like, for example, the blood compatibility is improved through physical coating, or the adsorption capacity is improved through chemical reaction immobilization. However, since most of the substrates used for the production of the conventional blood purification materials are porous materials such as carbonized resins and adsorbent resins, and these materials are usually cross-linked and have few groups capable of being modified, when the porous materials such as carbonized resins and adsorbent resins are directly coated with polyvinyl butyral (PVB), the resulting coating film has a low adsorption force to the substrates and is easily detached.
Disclosure of Invention
The invention provides a blood purification material based on mussel bionic chemistry and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme.
The blood purification material based on mussel bionic chemistry comprises a porous adsorption base material, an adsorption layer and a coating film in sequence from inside to outside, wherein the adsorption layer is one or more of polymyxin B sulfate, polylysine hydrochloride, polyethyleneimine or polydopamine and is wound on the porous adsorption base material in a molecular chain form; the coating film is a polyvinyl butyral-gallic acid film or a polyvinyl butyral film.
Further, the porous adsorption substrate comprises activated carbon, adsorption resin, carbonized resin, polystyrene divinylbenzene microspheres, polymethacrylate microspheres, resin-based carbonized resin, asphalt-based carbonized resin, agarose microspheres, cellulose microspheres and a polyethylene porous sheet.
Furthermore, the aperture of the porous adsorption base material is 2-50 nm, and the specific surface area of the porous adsorption base material is more than 500m 2 /g。
Further, the polyvinyl butyral-gallic acid membrane is prepared from a mixed solution of polyvinyl butyral and gallic acid, wherein the polyvinyl butyral and the gallic acid are mixed in equal volume.
The preparation method of the blood purification material based on the mussel bionic chemistry comprises the following steps:
(1) coating one or more of polymyxin B sulfate solution, polylysine hydrochloride solution and polyethyleneimine solution on a porous adsorption substrate to form an adsorption layer;
(2) and (3) putting the porous adsorption base material with the adsorption layer into a mixed solution of polyvinyl butyral and gallic acid, wherein the pH value of the mixed solution of polyvinyl butyral and gallic acid is 8-10, the concentration of the polyvinyl butyral is 0.1-5%, and stirring for 12-36 h to finally obtain the mussel biomimetic chemistry-based blood purification material.
The preparation method of the blood purification material based on the mussel bionic chemistry comprises the following steps:
a. coating a polydopamine solution on a porous adsorption base material to form a polydopamine adsorption layer;
b. and (3) putting the porous adsorption base material with the polydopamine adsorption layer into a polyvinyl butyral solution, wherein the pH value of the polyvinyl butyral solution is 8-10, the concentration of the polyvinyl butyral is 0.1-5%, and stirring for 12-36 h to finally obtain the mussel biomimetic chemistry-based blood purification material.
Further, the mass fraction of the polymyxin B sulfate solution is 0.1-30%, the mass fraction of the polylysine hydrochloride solution is 0.1-30%, and the mass fraction of the polyethyleneimine solution is 0.1-30%.
Further, the mass fraction of the polydopamine solution is 0.1-30%.
Furthermore, the mole fraction ratio of the catechol group to the amido group in the polydopamine solution is 0.1-2.
Furthermore, the mole fraction ratio of the catechol group to the imino group in the polydopamine solution is 0.1-2.
The invention has the beneficial effects that: the mucus secreted by marine mussel organisms through byssus has super-strong waterproof adhesion and universal adhesion performances, and the research shows that the main component of the mucus is mussel adhesion protein, a large number of structures such as 3, 4-dihydroxy-L-phenylalanine (DOPA) residues, lysine residues, hydroxyproline residues and the like exist in amino acid fragments obtained by hydrolyzing the mussel adhesion protein, and at least 5 adhesion proteins containing DOPA exist in the protein secreted by the byssus of the marine mussel organisms, wherein the DOPA content in byssus adhesion protein-5 (Mefp-5) and byssus adhesion protein-3 (Mefp-3) distributed at the interface between the byssus adhesion disc and the substrate is higher, and the molar fraction of the dopis up to 30%; further research on DOPA shows that DOPA has a catechol group (also called catechol) which has a plurality of chemical multifunctionalities and affinity diversity, the group is easily oxidized into quinone under the condition of increasing pH value, the adhesion mechanism of DOPA is more complicated due to the introduction of the quinone structure, the interaction between the group and the surface of the organic substrate is realized through an irreversible covalent bond, and thus the DOPA can be strongly adhered to the organic substrate;
therefore, in the technical scheme of the invention, the gallic acid solution of the polyvinyl butyral is used as a coating material, the gallic acid solution of the polyvinyl butyral is rich in catechol group, polymyxin B sulfate (PMB), polylysine hydrochloride (PLL) or Polyethyleneimine (PEI) is rich in amino and imino, so that the gallic acid of the polyvinyl butyral and the adsorption layer solution rich in amino and imino can simulate the structure of byssus secreted by marine mussels, and the polyvinyl butyral has excellent viscosity; the porous adsorption material is coated with one of polymyxin B sulfate solution, polylysine hydrochloride solution and polyethyleneimine solution to form an adsorption layer, the adsorption layer can be entangled in a porous structure of a cross-linked porous material matrix and is cross-linked with PVB to form an interpenetrating polymer network structure with the porous material matrix to form an interpenetrating polymer network polymer, the PVB coating and the porous adsorption substrate have no chemical bond effect, the movement range of the PVB coating and the porous adsorption substrate is limited only by the interpenetrating polymer network structure, so that the PVB film layer is not easy to fall off, and the stability of the material is improved.
Drawings
FIG. 1 is a graph showing ultraviolet absorption spectra of the blood purification material obtained in example 1 and the blood purification material obtained in comparative example.
Detailed Description
Example 1
A blood purification material based on mussel bionic chemistry comprises a porous adsorption base material, an adsorption layer and a coating film in sequence from inside to outside, wherein the adsorption layer is a polylysine hydrochloride adsorption layer, and polylysine hydrochloride is wound on the porous adsorption base material in a molecular chain form; the coating film is a polyvinyl butyral-gallic acid film; the porous adsorption base material is carbonized resin.
The preparation method of the blood purification material comprises the following steps:
(1) coating a polylysine hydrochloride solution on a carbonized resin to form a polylysine hydrochloride adsorption layer, wherein the mass fraction of the polylysine hydrochloride solution is 20%, the pore diameter of the carbonized resin is 2-50 nm, and the specific surface area of a porous adsorption base material is more than 500m 2 /g；
(2) Putting the carbonized resin attached with the polylysine hydrochloride adsorption layer into a mixed solution of polyvinyl butyral and gallic acid, wherein the volume of the mixed solution is equal to that of the polyvinyl butyral and the gallic acid, the concentration of the polyvinyl butyral is 0.6%, the pH value of the mixed solution is 8.5, stirring for 24h, taking out the mixed solution, and cleaning the mixed solution with alcohol and water for injection to obtain the blood purification material based on the mussel biomimetic chemistry.
Example 2
A blood purification material based on mussel bionic chemistry comprises a porous adsorption base material, an adsorption layer and a coating film in sequence from inside to outside, wherein the adsorption layer is a polymyxin B sulfate adsorption layer, and polymyxin B sulfate is wound on the porous adsorption base material in a molecular chain form; the coating film is a polyvinyl butyral-gallic acid film; the porous adsorption base material is carbonized resin.
The preparation process of the blood purification material comprises the following steps:
(1) coating a polymyxin B (PMB) sulfate solution on carbonized resin to form a polymyxin B sulfate adsorption layer, wherein the mass fraction of the polymyxin B sulfate solution is 5%, the pore diameter of the carbonized resin is 2-50 nm, and the specific surface area of a porous adsorption base material is more than 500m 2 /g；
(2) Putting the carbonized resin attached with the polymyxin B sulfate adsorption layer into a mixed solution of polyvinyl butyral and gallic acid, wherein the volume of the mixed solution is equal to that of the polyvinyl butyral and the gallic acid, the concentration of the polyvinyl butyral is 1%, the pH value of the mixed solution is 8.0, stirring for 24h, taking out the mixed solution, and cleaning the mixed solution with alcohol and water for injection to obtain the blood purification material based on the mussel biomimetic chemistry.
Example 3
A blood purification material based on mussel bionic chemistry comprises a porous adsorption base material, an adsorption layer and a coating film in sequence from inside to outside, wherein the adsorption layer is polyethyleneimine, and the polyethyleneimine is wound on the porous adsorption base material in a molecular chain form; the coating film is a polyvinyl butyral-gallic acid film, and the porous adsorption substrate is polystyrene divinyl adsorption resin.
The preparation process of the blood purification material comprises the following steps:
(1) coating a polyethyleneimine solution on polystyrene divinylbenzene adsorption resin to form a polyethyleneimine adsorption layer on the polystyrene divinylbenzene adsorption resin, wherein the mass fraction of the polyethyleneimine solution is 10%, the pore diameter of the polystyrene divinylbenzene adsorption resin is 2-50 nm, and the specific surface area of the polystyrene divinylbenzene adsorption resin is more than 500m 2 /g；
(2) Putting the polystyrene divinyl benzene adsorption resin with the attached polyethyleneimine adsorption layer into a mixed solution of polyvinyl butyral and gallic acid, wherein the volume of the polyvinyl butyral and the gallic acid is equal to one volume, the concentration of the polyvinyl butyral is 1.5%, the pH value of the mixed solution is 9.0, stirring for 24 hours, covering a polyvinyl butyral-gallic acid film on the surface of the polystyrene divinyl benzene adsorption resin, taking out the polystyrene divinyl benzene adsorption resin, and cleaning the polystyrene divinyl benzene adsorption resin with alcohol and water for injection to obtain the mussel biomimetic chemistry-based blood purification material.
Example 4
A blood purification material based on mussel bionic chemistry comprises a porous adsorption base material, an adsorption layer and a coating film in sequence from inside to outside, wherein the adsorption layer is filled with polydopamine, and the polydopamine is wound on the porous adsorption base material in a molecular chain form; the coating film is a polyvinyl butyral film, and the porous adsorption base material is carbonized resin.
The preparation process of the blood purification material comprises the following steps:
(1) coating a polydopamine solution on carbonized resin to form a polydopamine adsorption layer on the carbonized resin, wherein the mass fraction of the polydopamine solution is 25%, the pore diameter of the carbonized resin is 2-50 nm, and the specific surface area of the carbonized resin is more than 500m 2 /g；
(2) And (3) putting the carbonized resin with the poly dopamine adsorption layer into a polyvinyl butyral solution, wherein the concentration of the polyvinyl butyral solution is 0.4%, adjusting the pH value of the mixed solution to 10.0, stirring for 24 hours, then coating a polyvinyl butyral film on the surface of the carbonized resin, taking out the carbonized resin, and cleaning the carbonized resin with alcohol and water for injection to obtain the blood purification material based on the mussel biomimetic chemistry.
Comparative example
And (3) putting the carbonized resin into a polyvinyl butyral solution, carrying out physical coating on the polyvinyl butyral solution with the mass fraction of 0.6%, and then cleaning the film by using water for injection.
The blood purification materials prepared in example 1 and comparative example were subjected to a plasma adsorption experiment, and 1mL of the blood purification materials prepared in example 1 and comparative example were taken, respectively, and then added to the plasma of a patient, respectively, at a temperature of 37 ℃ and a shaking adsorption time of 2 hours with a shaking rate of 60 ± 10rpm, after which the concentration of toxins in the plasma of the patient was measured, and the clearance rates of the blood purification materials prepared in example 1 and comparative example were calculated, respectively, as shown in table 1.
Table 1 clearance of blood purifying materials prepared in example 1 and comparative example
Through the data in table 1, when the blood purification material prepared in example 1 is compared with the blood purification material prepared in the comparative example, the blood purification material prepared in example 1 has greatly improved performance of removing toxins such as total bilirubin and endotoxin, and the removal rate can reach more than 50%.
The blood purification material prepared in example 1 and the blood purification material prepared in comparative example were separately packed in adsorption column containers under the same conditions, and distilled water was injected thereto, followed by a high temperature and high pressure sterilization test. After the high temperature and high pressure sterilization test is completed, the solution in the adsorption vessel is detected to obtain an ultraviolet absorption spectrogram, which is shown in fig. 1. It can be seen from fig. 1 that the absorbance of the solution in the comparative example is greater than that of the solution in example 1, which indicates that the blood purification material prepared in the comparative example is subjected to the autoclaving treatment, and the coating film thereon is more peeled off, resulting in a large absorbance; after the blood purification material prepared in the embodiment 1 is subjected to high-temperature and high-pressure sterilization treatment, the coating film of the blood purification material basically falls off less, so that the absorbance of the solution is lower and gentle; therefore, the blood purification material prepared by the method has higher bonding strength and is not easy to fall off compared with the blood purification material prepared by the traditional method.
The blood purification materials prepared in examples 1 to 4 were subjected to hemolysis rate measurement according to test selection on interaction with blood in part 4 of GB/T16886.4-2003 medical device biological evaluation and test method of GB/T14233.2-2005 part 2 of medical transfusion, blood transfusion, and injection device test methods: the hemolysis rates of the samples obtained in examples 1-4 were 3.7%, 3.6%, 3.8% and 3.7%, respectively, and all of them were less than 5% according to the national standard.
Blood compatibility tests were performed on the blood prepared in examples 1 to 4, and 1mL of the blood purification material prepared in examples 1 to 4 was taken, soaked in physiological saline for 10 hours, sealed in a container for sterilization, and then injected with 10mL of rabbit whole blood by using a syringe, wherein the injected rabbit whole blood was anticoagulated with heparin sodium, and then flowed at a flow rate of 50mL/min for 2 hours. The change in each component of blood before and after the flow was measured by a hemocyte analyzer.
The results show that the main components in the blood do not change much before and after the blood purification materials prepared in the examples 1 to 4 flow, and the reduction percentage is basically about 11%, so that the mussel biomimetic chemical blood purification material prepared by the invention has good blood compatibility.
Claims (8)
1. The mussel biomimetic chemistry-based blood purification material is characterized by comprising a porous adsorption substrate, an adsorption layer and a coating film in sequence from inside to outside, wherein the adsorption layer is one or more of polymyxin B sulfate, polylysine hydrochloride, polyethyleneimine or polydopamine and is wound on the porous adsorption substrate in a molecular chain form; the coating film is a polyvinyl butyral-gallic acid film or a polyvinyl butyral film;
the aperture of the porous adsorption base material is 2-50 nm, and the specific surface area of the porous adsorption base material is more than 500m 2 /g；
The polyvinyl butyral-gallic acid film is prepared from a mixed solution of polyvinyl butyral and gallic acid, wherein the volume of the polyvinyl butyral and the gallic acid is equal to the volume of the mixed solution.
2. A mussel biomimetic chemistry based blood purification material according to claim 1, wherein the porous adsorption substrate comprises activated carbon, adsorption resin, charring resin, polystyrene divinylbenzene microspheres, polymethacrylate microspheres, resin-based charring resin, pitch-based charring resin, agarose microspheres, cellulose microspheres, polyethylene porous sheet.
3. The method for preparing a blood purification material based on mussel biomimetic chemistry according to claim 1, comprising the steps of:
(1) coating one or more of polymyxin B sulfate solution, polylysine hydrochloride solution and polyethyleneimine solution on a porous adsorption substrate to form an adsorption layer;
(2) and (3) putting the porous adsorption base material with the adsorption layer into a mixed solution of polyvinyl butyral and gallic acid, wherein the pH value of the mixed solution of polyvinyl butyral and gallic acid is 8-10, the concentration of the polyvinyl butyral is 0.1-5%, and stirring for 12-36 h to finally obtain the mussel biomimetic chemistry-based blood purification material.
4. A method for preparing a mussel biomimetic chemistry based blood purification material according to claim 3, wherein the polymyxin B sulfate solution is 0.1-30% by mass, the polylysine hydrochloride solution is 0.1-30% by mass, and the polyethyleneimine solution is 0.1-30% by mass.
5. The method for preparing a blood purification material based on mussel biomimetic chemistry according to claim 1, comprising the steps of:
a. coating a polydopamine solution on a porous adsorption base material to form a polydopamine adsorption layer;
b. and (3) putting the porous adsorption base material with the polydopamine adsorption layer into a polyvinyl butyral solution, wherein the pH value of the polyvinyl butyral solution is 8-10, the concentration of the polyvinyl butyral is 0.1-5%, and stirring for 12-36 h to finally obtain the mussel biomimetic chemistry-based blood purification material.
6. The method for preparing a blood purification material based on mussel biomimetic chemistry according to claim 5, wherein the mass fraction of the polydopamine solution is 0.1-30%.
7. The method for preparing a blood purification material based on mussel biomimetic chemistry according to claim 5, wherein the molar fraction ratio of catechol groups to amine groups in the polydopamine solution is 0.1-2.
8. The method for preparing a blood purification material based on mussel biomimetic chemistry according to claim 5, wherein the molar fraction ratio of catechol groups to imino groups in the polydopamine solution is 0.1-2.
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