CN108498859B - Antibacterial bioactive glass nanofiber scaffold and preparation method thereof - Google Patents
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Abstract
The invention belongs to the field of biological functional materials, and discloses a preparation method of an antibacterial bioactive glass nanofiber scaffold, which comprises the following steps: and respectively carrying out chemical reaction on the pure bacterial cellulose film in ceric ammonium nitrate and ethylenediamine solutions to graft amino on hydroxyl of the bacterial cellulose, so as to obtain the aminated modified bacterial cellulose. Then taking the aminated bacterial cellulose as a template, and carrying out ultrasonic treatment on AgNO containing the antibacterial component3Depositing on the nano-fiber and respectively depositing a precursor containing Ca and Si elements on the surface of the superfine nano-fiber, calcining to prepare the antibacterial bioglass scaffold with the superfine nano-scale network structure, and rapidly inducing the formation of hydroxyapatite by virtue of the unique three-dimensional network structure. The invention has the advantages of simple process, low cost of raw materials and the like, and the obtained biological glass nanofiber scaffold has good antibacterial performance and high biological activity and has good application prospect.
Description
Technical Field
The invention belongs to the field of biological functional materials, and particularly relates to an antibacterial bioactive glass nanofiber scaffold and a preparation method thereof.
Background
Scientists have been working on various studies to ensure the quality of life of humans. Bones, which are important tissue organs of the human body, assume the critical role of maintaining normal physiological activities, but also face inevitably serious health problems. As a representative example of bone replacement and bone graft materials, bioactive glass has a strong expression in bone tissue regeneration, has good biocompatibility, bioactivity, osteoconductivity and osteoinductivity, receives more and more attention, and has a very important meaning for sufficient development and utilization of the bioactive glass.
So far, a great deal of research reports that bioglass with high specific surface area and porosity has higher bioactivity and good biomimetic mineralization performance, and after being soaked in Simulated Body Fluid (SBF) for a period of time, bone-like hydroxyapatite carbonate crystals can be generated on the surface of the bioglass, which is one of the most important standards for judging whether the material has bioactivity. But the high porosity can improve the bioactivity and provide an ideal proliferation place for harmful microorganisms such as bacteria, and the like, and the long-term implantation of the biomedical material into a human body can cause the adhesion of the microorganisms such as bacteria and the like on the surface of the biomedical material, thereby causing infection. With the wide application of human implantation medical devices such as artificial bone scaffolds, dental implants and the like, bacterial infectious diseases generated by medical devices have become one of the important issues of clinical laboratories. Recent studies have shown that loading a surface antibiotic coating has a good short-term effect against post-operative infections. However, the antibiotics are difficult to accurately locate and release in the human body. In addition, high concentrations of antibiotics increase the risk of systemic toxicity, and antibiotic coatings also promote the development of bacterial resistance. Therefore, implant materials are designed with consideration of not only biocompatibility and osseointegration ability but also antibacterial properties. The infection phenomenon after the bioglass material is implanted into a human body not only brings serious health threat and heavy economic burden to human beings, but also limits the application and development of biomedical materials to a certain extent. At present, the preparation scale of the biological glass bracket at home and abroad is mainly concentrated between a micropore and a macropore, the prepared biological material has smaller specific surface area and lower biological activity, and if postoperative infection is overcome by injecting antibiotics after implantation, the physical burden and the economic burden of a patient are undoubtedly increased, and meanwhile, the great demand of human tissue engineering on the biological glass material is difficult to meet.
The bacterial cellulose has a superfine three-dimensional network structure, has huge three-dimensional space outside the nano-fiber, is easy to contain water, alcohols, inorganic substances, organic matter precursors and other solutions or sol particles and the like, provides conditions for the deposition of a target object on the surface of the bacterial cellulose, and is widely applied to the field of biological nano-functional materials due to the nanoscale pore diameter and the larger specific surface area of the bacterial cellulose. Silver (Ag) and silver ion (Ag)+) It has long been known that the substance has the most effective antibacterial effect against bacteria, viruses, algae and fungi, and has multiple bactericidal mechanisms such as inhibition of the respiratory chain of cells, alteration of the permeability of cell membranes, and denaturation of nucleic acids. However, because the surface hydroxyl of the bacterial cellulose has low chemical activity and is difficult to combine with silver ions and other components in general, the method for performing amination modification on the bacterial cellulose is adopted, so that the chemical active sites of the bacterial cellulose are increased, and the combining capability of the cellulose on the silver ions and other cations is greatly improved.
According to the invention, by means of the superfine network structure of bacterial cellulose, the silver-doped biological glass nanofiber scaffold with the superfine nano network structure is obtained by calcining after biological glass precursor components containing calcium and silicon and Ag with an antibacterial effect are deposited. The method provides a new path for preparing the antibacterial biological glass nanofiber scaffold, and has certain practical significance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the nano glass fiber scaffold with simple operation process, three-dimensional superfine network structure, high specific surface area and high biological activity and the preparation method thereof, aiming at improving the binding capacity of cellulose nano fibers to biological glass precursor components by carrying out amination modification on bacterial cellulose so as to prepare the inorganic nano fiber biological glass scaffold with the nano network structure.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an antibacterial bioactive glass nanofiber scaffold comprises the steps of taking aminated bacterial cellulose as an organic template, depositing a biological glass precursor component containing calcium and silicon and Ag with an antibacterial effect on the organic template, and calcining to obtain the silver-doped biological glass nanofiber scaffold with a superfine nano network structure.
The preparation method of the antibacterial bioactive glass nanofiber scaffold comprises the following specific steps:
(1) preparing aminated bacterial cellulose;
(2) deposition of a calcium-containing precursor: adding 0.1-1 mol/L Ca (NO) into the aminated bacterial cellulose3)2·4H2Performing ultrasonic treatment for 3 h in ethanol solution of O, wherein the calcium-containing solution is replaced every 1 h;
(3) deposition of Ag: putting the aminated bacterial cellulose treated in the step (2) into 0.1-1 mol/L AgNO3The ethanol solution is subjected to ultrasonic treatment for 3 hours, wherein the silver-containing solution is replaced every 1 hour;
(4) deposition of a silicon-containing precursor: putting the aminated bacterial cellulose treated in the step (3) into a mixed solution of tetraethyl orthosilicate and absolute ethyl alcohol according to the volume ratio of 1:40, continuing to perform ultrasonic treatment for 3 hours, changing the silicon-containing solution every 1 hour, continuously cleaning with deionized water after the ultrasonic treatment is finished, dissolving the cleaned aminated bacterial cellulose in a solvent, and performing freeze drying;
(5) calcining the aminated bacterial cellulose block obtained after freeze drying at 600-800 ℃ for 1-3 h to obtain a calcined product, namely the bioactive glass nanofiber scaffold.
The solvent in the step (4) is one or two of tert-butyl alcohol and water.
The temperature rise rate of the calcination in the step (5) is 5-20 ℃/min.
The preparation of the aminated bacterial cellulose in the step (1) specifically comprises the following steps:
1) shearing a bacterial cellulose film into blocks, soaking the blocks in 0.5-2 mol/L NaOH solution at 90 ℃ for 2-5 h, washing the blocks with deionized water to be neutral, dissolving the washed bacterial cellulose in a solvent, and freeze-drying the solution in a freeze dryer to obtain a bacterial cellulose block;
2) putting the bacterial cellulose block into constant-temperature water introduced at 35 ℃, continuously introducing nitrogen to remove oxygen dissolved in the water, adding a ceric ammonium nitrate solution with the concentration of 0.1 mol/L to react for 15 min, then continuously dripping poly glycidyl methacrylate GMA for 30 min, washing the bacterial cellulose block with deionized water after reacting for 2 h, washing the bacterial cellulose block with absolute ethyl alcohol, repeatedly washing the bacterial cellulose block to be neutral to obtain a white block, dissolving the white block into a solvent, and then freeze-drying the white block; wherein the mass ratio of the bacterial cellulose to the ammonium ceric nitrate to the GMA is 1:20: 2;
3) putting the white block obtained in the step 2) into a mixed solution prepared from ethylenediamine and water according to the mass ratio of 3:2, stirring for 2 hours at 80 ℃, washing with deionized water once, washing with absolute ethyl alcohol once, repeatedly washing to neutrality in the way to obtain the aminated bacterial cellulose, dissolving the aminated bacterial cellulose in a solvent, and freeze-drying to obtain the aminated bacterial cellulose.
The solvent in the step 1), the step 2) and the step 3) is one or two of tert-butyl alcohol and water.
The ammonium ceric nitrate solution in the step 2) is prepared by dissolving ammonium ceric nitrate in 1 mol/L HNO3In aqueous solution.
The antibacterial bioactive glass nanofiber scaffold prepared by the preparation method is provided.
Compared with the prior art, the invention has the following advantages:
1. the preparation process is simple to operate, low in time consumption and capable of completing the preparation process in a short time.
2. According to the invention, through carrying out amination modification on bacterial cellulose and adopting an ultrasonic method, the binding capacity of the components of the biological glass precursor and silver on the bacterial cellulose nanofiber is improved, and the antibacterial biological glass nanofiber scaffold with the superfine nano network structure is prepared. The prepared organismThe porosity of the active glass nanofiber bracket reaches 79 percent, and the specific surface area reaches 144.6g/m2The antibacterial rate of the antibacterial agent to staphylococcus aureus reaches 97%, and the antibacterial agent can induce the generation of hydroxyapatite after being soaked in simulated body fluid for 24 hours, thereby showing good biological activity. The method provides a new path for preparing the antibacterial biological glass nanofiber scaffold, and has certain practical significance.
Drawings
FIG. 1 is an SEM image of aminated bacterial cellulose of the present invention;
FIG. 2 is an SEM image of aminated bacterial cellulose with calcium, silicon, and silver deposited on the surface thereof in example 1 of the present invention;
FIG. 3 is an SEM image of aminated bacterial cellulose after deposition of Ca, Si, and Ag, and calcination at 700 deg.C in example 3 of the present invention.
Detailed description of the invention
The technical solution of the present invention will be described in detail by examples, but the present invention is not limited thereto.
Example 1
A preparation method of an antibacterial bioactive glass nanofiber scaffold comprises the following specific steps:
(1) shearing a bacterial cellulose film into blocks, soaking the blocks in 1 mol/L NaOH solution at 90 ℃ for 2 hours, then washing the blocks with a large amount of deionized water to be neutral, dispersing the washed bacterial cellulose in water, and freeze-drying the bacterial cellulose in a freeze dryer to obtain bacterial cellulose blocks;
(2) putting the bacterial cellulose block into constant-temperature water introduced at 35 ℃, continuously introducing nitrogen to remove oxygen dissolved in the water, adding a ceric ammonium nitrate solution with the concentration of 0.1 mol/L for reaction for 15 min, then continuously dripping polyglycidyl methacrylate GMA for 30 min, washing the bacterial cellulose block with deionized water after reacting for 2 h, washing the bacterial cellulose block with absolute ethyl alcohol, repeatedly washing the bacterial cellulose block to be neutral to obtain a white block, dispersing the white block into the water, and then freeze-drying the white block; wherein the mass ratio of the bacterial cellulose to the ammonium ceric nitrate to the GMA is 1:20: 2;
(3) putting the white block obtained in the step (2) into 125mL of mixed solution prepared from ethylenediamine and water according to the mass ratio of 3:2, stirring for 2 h at 80 ℃, finally cleaning according to the method in the step (2) to obtain aminated bacterial cellulose, dispersing the aminated bacterial cellulose in water, and freeze-drying;
(4) adding 0.1 mol/L Ca (NO) into the aminated cellulose according to the mass ratio of 1:1003)2·4H2Performing ultrasonic treatment for 3 h in ethanol solution of O, wherein the calcium-containing solution is replaced every 1 h;
(5) putting aminated cellulose into AgNO of 0.1 mol/L according to the mass ratio of 1:1003The ethanol solution is subjected to ultrasonic treatment for 3 hours, wherein the solution is replaced every 1 hour;
(6) putting the aminated bacterial cellulose block subjected to calcium deposition into a mixed solution of tetraethyl orthosilicate and absolute ethyl alcohol according to the volume ratio of 1:40, continuing to perform ultrasonic treatment for 3 hours, changing a silicon-containing solution every 1 hour, continuing to perform cleaning with deionized water after the ultrasonic treatment is completed, dispersing the cleaned bacterial cellulose in water, and performing freeze drying;
(7) and calcining the amination bacterial cellulose block obtained after final freeze drying at 700 ℃ for 1 h to obtain the bioactive glass nanofiber scaffold.
Example 2
A preparation method of an antibacterial bioactive glass nanofiber scaffold comprises the following specific steps:
(1) shearing a bacterial cellulose film into blocks, soaking the blocks in 1 mol/L NaOH solution at 90 ℃ for 2 h, then washing the blocks with a large amount of deionized water to be neutral, dispersing the washed bacterial cellulose in tert-butyl alcohol, and freeze-drying the blocks in a freeze dryer to obtain bacterial cellulose blocks;
(2) putting the bacterial cellulose block into constant-temperature water introduced at 35 ℃, continuously introducing nitrogen to remove oxygen dissolved in the water, adding a ceric ammonium nitrate solution with the concentration of 0.1 mol/L to react for 15 min, then continuously dripping poly glycidyl methacrylate GMA for 30 min, washing the bacterial cellulose block with deionized water after reacting for 2 h, washing the bacterial cellulose block with absolute ethyl alcohol, repeatedly washing the bacterial cellulose block to be neutral to obtain a white block, dispersing the white block into tert-butyl alcohol, and then freeze-drying the white block; wherein the mass ratio of the bacterial cellulose to the ammonium ceric nitrate to the GMA is 1:20: 2;
(3) putting the white block obtained in the step (2) into 125mL of mixed solution prepared from ethylenediamine and water according to the mass ratio of 3:2, stirring for 2 h at 80 ℃, finally cleaning according to the method in the step (2) to obtain aminated bacterial cellulose, dispersing the aminated bacterial cellulose in tert-butyl alcohol, and then carrying out freeze drying;
(4) adding 0.1 mol/L Ca (NO) into the aminated cellulose according to the mass ratio of 1:1003)2·4H2Performing ultrasonic treatment for 3 h in ethanol solution of O, wherein the calcium-containing solution is replaced every 1 h;
(5) putting aminated cellulose into AgNO of 0.1 mol/L according to the mass ratio of 1:1003The ethanol solution is subjected to ultrasonic treatment for 3 hours, wherein the solution is replaced every 1 hour;
(6) putting the aminated bacterial cellulose block subjected to calcium deposition into 125mL of mixed solution of tetraethyl orthosilicate and absolute ethyl alcohol according to the volume ratio of 1:40, continuing to perform ultrasonic treatment for 3 hours, changing the solution containing silicon every 1 hour, continuing to perform cleaning with deionized water after the ultrasonic treatment is finished, dispersing the cleaned bacterial cellulose into tert-butyl alcohol, and then performing freeze drying;
(7) and calcining the amination bacterial cellulose block obtained after final freeze drying at 700 ℃ for 1 h to obtain the bioactive glass nanofiber scaffold.
Example 3
A preparation method of an antibacterial bioactive glass nanofiber scaffold comprises the following specific steps:
(1) shearing a bacterial cellulose film into blocks, soaking the blocks in 1 mol/L NaOH solution at 90 ℃ for 2 h, then washing the blocks with a large amount of deionized water to be neutral, dispersing the washed bacterial cellulose in tert-butyl alcohol, and freeze-drying the blocks in a freeze dryer to obtain bacterial cellulose blocks;
(2) putting the bacterial cellulose block into constant-temperature water introduced at 35 ℃, continuously introducing nitrogen to remove oxygen dissolved in the water, adding a ceric ammonium nitrate solution with the concentration of 0.1 mol/L to react for 15 min, then continuously dripping poly glycidyl methacrylate GMA for 30 min, washing the bacterial cellulose block with deionized water after reacting for 2 h, washing the bacterial cellulose block with absolute ethyl alcohol, repeatedly washing the bacterial cellulose block to be neutral to obtain a white block, dispersing the white block into tert-butyl alcohol, and then freeze-drying the white block; wherein the mass ratio of the bacterial cellulose to the ammonium ceric nitrate to the GMA is 1:20: 2;
(3) putting the white block obtained in the step (2) into 125mL of mixed solution prepared from ethylenediamine and water according to the mass ratio of 3:2, stirring for 2 h at 80 ℃, finally cleaning according to the method in the step (2) to obtain aminated bacterial cellulose, dispersing the aminated bacterial cellulose in tert-butyl alcohol, and then freeze-drying;
(4) adding 0.1 mol/L Ca (NO) into the aminated cellulose according to the mass ratio of 1:1003)2·4H2Performing ultrasonic treatment for 3 h in ethanol solution of O, wherein the calcium-containing solution is replaced every 1 h;
(5) putting aminated cellulose into AgNO of 0.1 mol/L according to the mass ratio of 1:1003The ethanol solution is subjected to ultrasonic treatment for 3 hours, wherein the solution is replaced every 1 hour;
(6) putting the aminated bacterial cellulose block subjected to calcium deposition into a mixed solution of tetraethyl orthosilicate and absolute ethyl alcohol according to the volume ratio of 1:40, continuing to perform ultrasonic treatment for 3 hours, changing a silicon-containing solution every 1 hour, continuing to perform deionized water cleaning after the ultrasonic treatment is completed, and then performing freeze drying;
(7) and calcining the amination bacterial cellulose block subjected to calcium, silicon and silver deposition and finally obtained after freeze drying at 700 ℃ for 1 h to obtain the bioactive glass nanofiber scaffold.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (6)
1. A preparation method of an antibacterial bioactive glass nanofiber scaffold is characterized by comprising the following steps: depositing a biological glass precursor component containing calcium and silicon and Ag with an antibacterial effect on an organic template by taking the aminated bacterial cellulose as the organic template, and calcining to obtain a silver-doped biological glass nanofiber scaffold with an ultrafine nano network structure;
the preparation method comprises the following specific steps:
(1) preparing aminated bacterial cellulose;
(2) deposition of a calcium-containing precursor: adding 0.1-1 mol/L Ca (NO) into the aminated bacterial cellulose3)2·4H2Performing ultrasonic treatment for 3 h in ethanol solution of O, wherein the calcium-containing solution is replaced every 1 h;
(3) deposition of Ag: putting the aminated bacterial cellulose treated in the step (2) into 0.1-1 mol/L AgNO3The ethanol solution is subjected to ultrasonic treatment for 3 hours, wherein the silver-containing solution is replaced every 1 hour;
(4) deposition of a silicon-containing precursor: putting the aminated bacterial cellulose treated in the step (3) into a mixed solution of tetraethyl orthosilicate and absolute ethyl alcohol according to the volume ratio of 1:40, continuing to perform ultrasonic treatment for 3 hours, changing the silicon-containing solution every 1 hour, continuously cleaning with deionized water after the ultrasonic treatment is finished, dissolving the cleaned aminated bacterial cellulose in a solvent, and performing freeze drying;
(5) calcining the aminated bacterial cellulose block obtained after freeze drying at 600-800 ℃ for 1-3 h to obtain a calcined product, namely the bioactive glass nanofiber scaffold;
the preparation of the aminated bacterial cellulose in the step (1) specifically comprises the following steps:
1) shearing a bacterial cellulose film into blocks, soaking the blocks in 0.5-2 mol/L NaOH solution at 90 ℃ for 2-5 h, washing the blocks with deionized water to be neutral, dissolving the washed bacterial cellulose in a solvent, and freeze-drying the solution in a freeze dryer to obtain a bacterial cellulose block;
2) putting the bacterial cellulose block into constant-temperature water introduced at 35 ℃, continuously introducing nitrogen to remove oxygen dissolved in the water, adding a ceric ammonium nitrate solution with the concentration of 0.1 mol/L to react for 15 min, then continuously dripping poly glycidyl methacrylate GMA for 30 min, washing the bacterial cellulose block with deionized water after reacting for 2 h, washing the bacterial cellulose block with absolute ethyl alcohol, repeatedly washing the bacterial cellulose block to be neutral to obtain a white block, dissolving the white block into a solvent, and then freeze-drying the white block; wherein the mass ratio of the bacterial cellulose to the ammonium ceric nitrate to the GMA is 1:20: 2;
3) putting the white block obtained in the step 2) into 125mL of mixed solution prepared from ethylenediamine and water according to the mass ratio of 3:2, stirring for 2 h at 80 ℃, washing with deionized water once, washing with absolute ethyl alcohol once, repeatedly washing to neutrality in the way to obtain aminated bacterial cellulose, dissolving the aminated bacterial cellulose in a solvent, and freeze-drying to obtain the aminated bacterial cellulose.
2. The method for preparing an antibacterial bioactive glass nanofiber scaffold as claimed in claim 1, wherein the method comprises the following steps: the solvent in the step (4) is one or two of tert-butyl alcohol and water.
3. The method for preparing an antibacterial bioactive glass nanofiber scaffold as claimed in claim 1, wherein the method comprises the following steps: the temperature rise rate of the calcination in the step (5) is 5-20 ℃/min.
4. The method for preparing an antibacterial bioactive glass nanofiber scaffold as claimed in claim 1, wherein the method comprises the following steps: the solvent in the step 1), the step 2) and the step 3) is one or two of tert-butyl alcohol and water.
5. The method for preparing an antibacterial bioactive glass nanofiber scaffold as claimed in claim 1, wherein the method comprises the following steps: the ammonium ceric nitrate solution in the step 2) is prepared by dissolving ammonium ceric nitrate in 1 mol/L HNO3In aqueous solution.
6. An antibacterial bioactive glass nanofiber scaffold prepared by the preparation method as claimed in any one of claims 1 to 5.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102266583A (en) * | 2011-07-10 | 2011-12-07 | 东华大学 | Preparation method of silver-loading modified bacterial cellulose based compound functional wet dressing |
| WO2011150482A1 (en) * | 2010-05-31 | 2011-12-08 | Fundação De Amparo À Pesquisa Do Estado de São Paulo | Methods for obtaining reabsorbable composites, composites, membrane, scaffold and its uses |
| CN103301151A (en) * | 2013-05-14 | 2013-09-18 | 王林 | Silver-iodide-doped bioactive glass as well as preparation method and application of silver-iodide-doped bioactive glass |
| CN104707171A (en) * | 2015-02-03 | 2015-06-17 | 天津大学 | Preparation method of bioactive glass nanotube |
| CN105734718A (en) * | 2016-03-07 | 2016-07-06 | 北京科技大学 | Preparation method of multi-stage pore-size distribution material |
| CN106730017A (en) * | 2016-12-14 | 2017-05-31 | 广东省微生物研究所（广东省微生物分析检测中心） | A kind of sustained-release antibacterial composite membrane of bootable bone tissue regeneration and preparation method thereof |
-
2018
- 2018-03-30 CN CN201810293401.9A patent/CN108498859B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011150482A1 (en) * | 2010-05-31 | 2011-12-08 | Fundação De Amparo À Pesquisa Do Estado de São Paulo | Methods for obtaining reabsorbable composites, composites, membrane, scaffold and its uses |
| CN102266583A (en) * | 2011-07-10 | 2011-12-07 | 东华大学 | Preparation method of silver-loading modified bacterial cellulose based compound functional wet dressing |
| CN103301151A (en) * | 2013-05-14 | 2013-09-18 | 王林 | Silver-iodide-doped bioactive glass as well as preparation method and application of silver-iodide-doped bioactive glass |
| CN104707171A (en) * | 2015-02-03 | 2015-06-17 | 天津大学 | Preparation method of bioactive glass nanotube |
| CN105734718A (en) * | 2016-03-07 | 2016-07-06 | 北京科技大学 | Preparation method of multi-stage pore-size distribution material |
| CN106730017A (en) * | 2016-12-14 | 2017-05-31 | 广东省微生物研究所（广东省微生物分析检测中心） | A kind of sustained-release antibacterial composite membrane of bootable bone tissue regeneration and preparation method thereof |
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