银系纳米抗菌材料的制备与抗菌性能的研究
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摘要
随着科技的发展和人类生活水平的日益提高,人们对抗菌材料、抗菌制品的需求将会不断增加。为了增进人体健康,改善生活和工作环境,研究和开发新型、高效、无毒无味和抗菌性能持久的抗菌材料,成为当前的研究热点。银系抗菌材料具有高效、广谱、低毒、无味、不污染环境、安全环保等特点,正成为首选抗菌剂之一。
本论文研究了纳米银及载银纳米抗菌剂的制备工艺及其抗菌性能。分别用透射电子显微镜、扫描电子显微镜和原子力显微镜,紫外-可见吸收光谱、红外光谱,X射线衍射,X射线光电子能谱等技术对抗菌剂的表面形貌,光学特性,晶体结构和银的存在形态等进行了系统的表征。选用大肠杆菌和金黄色葡萄球菌两种菌种为代表,采用抑菌圈法、连续稀释法及SYNBIOSIS全自动微生物检测仪对制备的抗菌材料的抗菌性能进行了定性和定量检测。实验结果证实所制备的银系材料均对革兰氏阴性菌、革兰氏阳性菌及霉菌具有良好的抗菌性能。而且抗菌性能持久。
本论文由综述与实验两部分组成,全文共分七章。
第一章:对近年来抗菌剂的研究进展进行了全面的综述,对本领域今后的发展方向提出了展望。
第二章:以柠檬酸三钠、硼氢化钠为混和还原剂,采用化学还原法制备了不同的纳米银胶体,采用透射电镜对纳米银溶胶的形貌进行了表征,从而优化了制备条件,同时对纳米银溶胶的抗菌性等进行了研究。
第三章:利用化学还原法,用通过硝酸银、硼氢化钠和聚乙烯醇分别作为前驱体、还原剂和稳定剂,制备了均匀分散的银/聚乙烯醇纳米复合物溶胶,利用UV-Vis光谱,透射电子显微镜和原子力显微镜技术对纳米复合物的结构和形貌进行了系统的表征。分别以金黄色葡萄球菌、绿脓杆菌、大肠杆菌以及白色念珠菌为对象考察了纳米复合物溶胶对革兰氏阳性菌、革兰氏阴性菌和霉菌的抗菌活性。
第四章:利用化学还原法,以硝酸银、聚乙二醇分别作为前驱体、还原剂和稳定剂,制备了均匀分散的银/聚乙二醇纳米复合物溶胶,利用UV-Vis光谱,透射电子显微镜和原子力显微镜技术对纳米复合物的结构和形貌进行了系统的表征。分别以金黄色葡萄球菌、绿脓杆菌、大肠杆菌以及白色念珠菌考察了纳米复合物溶胶对革兰氏阳性菌、革兰氏阴性菌和霉菌的杀灭活性。本法以清洁无毒的聚乙二醇作为还原剂,以水作溶剂,是一种绿色无污染的制备方法。
第五章:采用浸渍法合成了纳米载银抗菌剂Ag/SiO_2,利用UV-Vis吸收光谱,X-射线粉末衍射,X射线光电子能谱、透射电子显微镜和原子力显微镜技术对纳米Ag/SiO_2的结构和形貌进行了系统的表征。分别以金黄色葡萄球菌、大肠杆菌为代表考察了纳米Ag/SiO_2对革兰氏阳性菌、革兰氏阴性菌的杀灭活性,发现纳米Ag/SiO_2对它们具有强的杀灭作用。
第六章:分别采用两步法和一步法合成了载银纳米介孔材料Ag/MCM-41,利用UV-Vis吸收光谱,X射线粉末衍射,低温氮气吸附,FT-IR,X射线光电子能谱、透射电子显微镜和原子力显微镜技术对纳米Ag/MCM-41的结构和形貌进行了系统的表征。研究结果表明,该类抗菌剂对以金黄色葡萄球菌、大肠杆菌为代表的革兰氏阳性菌、革兰氏阴性菌有很高的的抗菌活性,且作用持久。
第七章:采用两步法合成了纳米Ag/SBA-15,利用UV-Vis吸收光谱,X-射线粉末衍射,FT-IR,X射线光电子能谱、透射电子显微镜和原子力显微镜技术对纳米Ag/SBA-15的结构和形貌进行了系统的表征。分别以金黄色葡萄球菌、大肠杆菌为代表考察了纳米Ag/SBA-15对革兰氏阳性菌、革兰氏阴性菌的抗菌作用,性能良好。
With development of modern science and technology and progress of the society, the demands of people to antibacterial materials will enhance rapidly. It has become an important study topic and attracted a lot of attention in the past years to explore and develop new-type anti-bacterium materials with high efficiency, innocuity and lasting anti-bacterium capacity to control and restrain the growth and reproduction of deleterious bacteria. Due to some notable advantages such as high efficiency, broad-spectrum, low toxin , tastelessness and non-pollution, the silver-based antimicrobial agents has become a preferred field in antibacterial research.
The preparations of nanometric silver sols and silver-loaded antimicrobials and their antibacterial activities were studied in this thesis. The morphologies of the antimicrobials were characterized by transmission electron microscope(TEM), scanning electron microscope(SEM) and atomic force microscope (AFM), the optical characteristics were analyzed by ultraviolet-visible spectroscopy(UV-Vis spectra) and Fourier transform infrared spectroscopy(FT-IRs), the structures were evaluated by X-ray diffraction (XRD) and the chemical states of silver in matrix antimicrobials were investigated by X-ray photoelectron spectrum (XPS). The antibacterial activities of the antimicrobials and antibacterial products were characterized by inhibition zone, dilution and immersion. Escherichia coli (E.coli, ATCC25922), Peudomonas eruginosa (P. eruginosa, ATCC27853), Staphylococcus aureus (S. aureus, ATCC25923) and Candida albicans (C. albicans) are employed as models. These as-prepared materrials are proved to have good and long-lived antiseptic property to Gram-positive, Gam-negative bacteria and mildew.
The dissertation consists of seven parts:
In Chapter 1, a review on an investigation progress of the silver-based anti-bacterial materials has been described.
In chapter 2, Ag colloids were prepared by reduction method, in which the silver nitrate, sodium borohydride and tri-sodium citrate, and PVP served as precursor, reductant and stabilizer, respectively. The synthesized colloids have potent antibacterial activity toward both gram-positive and gram-negative bacteria. Further studies demonstrated that the Ag nanoparticle distribution was uniform by UV-Vis spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM) and atom force microscopy (AFM).
In chapter 3, Ag/PVA nanocomposites were prepared by in situ reduction method, in which the silver nitrate, sodium borohydride and poly (vinyl alcohol) (PVA) acted as precursor, reductant and stabilizer, respectively. The synthesized composites have a high antibacterial activity toward both gram-positive and gram-negative bacteria. PVA molecules effectively protected silver nanoparticles to avoid aggregation of the particles so that prepared silver nanopartilces were of small grain size, well-dispersive and stable in aqueous solution.
In chapter 4, stable Ag colloids were prepared by a simple process with polyethylene glycol (PEG) as an environmentally benign reducing agent and stabilizer, with water as green solvent. The structural and spectral analyses have showed a uniform size distribution with an average grain size less than 10 nm. The PEG-stablized colloids showed a high antibacterial activity toward gram-positive, gram-negative bacteria and fungi.
In chapter 5, the stable Ag/SiO_2 nanocomposites were prepared simply by an immersion method. The Ag/SiO_2 nanocomposites were characterized by UV–vis spectra, transmission electron microscopy (TEM) and atom force microscopy (AFM). The antibacterial experiments demonstrated the nanoparticles had a high and long-lived antibacterial activity toward gram-positive and gram-negative bacteria.
In chapter 6, the mesoporous nanocomposites Ag/MCM-41 were prepared respectively by a one-route procedure and a two-route one. Structural analyses have showed that nanoscale silver particles uniformly distributed inner the holes and on the surface of MCM-41 matrix. High antibacterial activities toward gram-positive and gram-negative bacteria attributed to conjunct actions of Ag+ ion and silver nanoparticles.
In chapter 7, the mesoporous Ag/SBA-15 nanocomposites were prepared by a two-step procedure. The Ag/SBA-15 nanocomposites were systemically characterized by UV–vis spectra, transmission electron microscopy (TEM), atom force microscopy (AFM) and so on. The antibacterial activity of the Ag/SBA-15 nanocomposites was also studied. The results showed that the sample has high antibacterial activity toward gram-positive and gram-negative.
本论文研究了纳米银及载银纳米抗菌剂的制备工艺及其抗菌性能。分别用透射电子显微镜、扫描电子显微镜和原子力显微镜,紫外-可见吸收光谱、红外光谱,X射线衍射,X射线光电子能谱等技术对抗菌剂的表面形貌,光学特性,晶体结构和银的存在形态等进行了系统的表征。选用大肠杆菌和金黄色葡萄球菌两种菌种为代表,采用抑菌圈法、连续稀释法及SYNBIOSIS全自动微生物检测仪对制备的抗菌材料的抗菌性能进行了定性和定量检测。实验结果证实所制备的银系材料均对革兰氏阴性菌、革兰氏阳性菌及霉菌具有良好的抗菌性能。而且抗菌性能持久。
本论文由综述与实验两部分组成,全文共分七章。
第一章:对近年来抗菌剂的研究进展进行了全面的综述,对本领域今后的发展方向提出了展望。
第二章:以柠檬酸三钠、硼氢化钠为混和还原剂,采用化学还原法制备了不同的纳米银胶体,采用透射电镜对纳米银溶胶的形貌进行了表征,从而优化了制备条件,同时对纳米银溶胶的抗菌性等进行了研究。
第三章:利用化学还原法,用通过硝酸银、硼氢化钠和聚乙烯醇分别作为前驱体、还原剂和稳定剂,制备了均匀分散的银/聚乙烯醇纳米复合物溶胶,利用UV-Vis光谱,透射电子显微镜和原子力显微镜技术对纳米复合物的结构和形貌进行了系统的表征。分别以金黄色葡萄球菌、绿脓杆菌、大肠杆菌以及白色念珠菌为对象考察了纳米复合物溶胶对革兰氏阳性菌、革兰氏阴性菌和霉菌的抗菌活性。
第四章:利用化学还原法,以硝酸银、聚乙二醇分别作为前驱体、还原剂和稳定剂,制备了均匀分散的银/聚乙二醇纳米复合物溶胶,利用UV-Vis光谱,透射电子显微镜和原子力显微镜技术对纳米复合物的结构和形貌进行了系统的表征。分别以金黄色葡萄球菌、绿脓杆菌、大肠杆菌以及白色念珠菌考察了纳米复合物溶胶对革兰氏阳性菌、革兰氏阴性菌和霉菌的杀灭活性。本法以清洁无毒的聚乙二醇作为还原剂,以水作溶剂,是一种绿色无污染的制备方法。
第五章:采用浸渍法合成了纳米载银抗菌剂Ag/SiO_2,利用UV-Vis吸收光谱,X-射线粉末衍射,X射线光电子能谱、透射电子显微镜和原子力显微镜技术对纳米Ag/SiO_2的结构和形貌进行了系统的表征。分别以金黄色葡萄球菌、大肠杆菌为代表考察了纳米Ag/SiO_2对革兰氏阳性菌、革兰氏阴性菌的杀灭活性,发现纳米Ag/SiO_2对它们具有强的杀灭作用。
第六章:分别采用两步法和一步法合成了载银纳米介孔材料Ag/MCM-41,利用UV-Vis吸收光谱,X射线粉末衍射,低温氮气吸附,FT-IR,X射线光电子能谱、透射电子显微镜和原子力显微镜技术对纳米Ag/MCM-41的结构和形貌进行了系统的表征。研究结果表明,该类抗菌剂对以金黄色葡萄球菌、大肠杆菌为代表的革兰氏阳性菌、革兰氏阴性菌有很高的的抗菌活性,且作用持久。
第七章:采用两步法合成了纳米Ag/SBA-15,利用UV-Vis吸收光谱,X-射线粉末衍射,FT-IR,X射线光电子能谱、透射电子显微镜和原子力显微镜技术对纳米Ag/SBA-15的结构和形貌进行了系统的表征。分别以金黄色葡萄球菌、大肠杆菌为代表考察了纳米Ag/SBA-15对革兰氏阳性菌、革兰氏阴性菌的抗菌作用,性能良好。
With development of modern science and technology and progress of the society, the demands of people to antibacterial materials will enhance rapidly. It has become an important study topic and attracted a lot of attention in the past years to explore and develop new-type anti-bacterium materials with high efficiency, innocuity and lasting anti-bacterium capacity to control and restrain the growth and reproduction of deleterious bacteria. Due to some notable advantages such as high efficiency, broad-spectrum, low toxin , tastelessness and non-pollution, the silver-based antimicrobial agents has become a preferred field in antibacterial research.
The preparations of nanometric silver sols and silver-loaded antimicrobials and their antibacterial activities were studied in this thesis. The morphologies of the antimicrobials were characterized by transmission electron microscope(TEM), scanning electron microscope(SEM) and atomic force microscope (AFM), the optical characteristics were analyzed by ultraviolet-visible spectroscopy(UV-Vis spectra) and Fourier transform infrared spectroscopy(FT-IRs), the structures were evaluated by X-ray diffraction (XRD) and the chemical states of silver in matrix antimicrobials were investigated by X-ray photoelectron spectrum (XPS). The antibacterial activities of the antimicrobials and antibacterial products were characterized by inhibition zone, dilution and immersion. Escherichia coli (E.coli, ATCC25922), Peudomonas eruginosa (P. eruginosa, ATCC27853), Staphylococcus aureus (S. aureus, ATCC25923) and Candida albicans (C. albicans) are employed as models. These as-prepared materrials are proved to have good and long-lived antiseptic property to Gram-positive, Gam-negative bacteria and mildew.
The dissertation consists of seven parts:
In Chapter 1, a review on an investigation progress of the silver-based anti-bacterial materials has been described.
In chapter 2, Ag colloids were prepared by reduction method, in which the silver nitrate, sodium borohydride and tri-sodium citrate, and PVP served as precursor, reductant and stabilizer, respectively. The synthesized colloids have potent antibacterial activity toward both gram-positive and gram-negative bacteria. Further studies demonstrated that the Ag nanoparticle distribution was uniform by UV-Vis spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM) and atom force microscopy (AFM).
In chapter 3, Ag/PVA nanocomposites were prepared by in situ reduction method, in which the silver nitrate, sodium borohydride and poly (vinyl alcohol) (PVA) acted as precursor, reductant and stabilizer, respectively. The synthesized composites have a high antibacterial activity toward both gram-positive and gram-negative bacteria. PVA molecules effectively protected silver nanoparticles to avoid aggregation of the particles so that prepared silver nanopartilces were of small grain size, well-dispersive and stable in aqueous solution.
In chapter 4, stable Ag colloids were prepared by a simple process with polyethylene glycol (PEG) as an environmentally benign reducing agent and stabilizer, with water as green solvent. The structural and spectral analyses have showed a uniform size distribution with an average grain size less than 10 nm. The PEG-stablized colloids showed a high antibacterial activity toward gram-positive, gram-negative bacteria and fungi.
In chapter 5, the stable Ag/SiO_2 nanocomposites were prepared simply by an immersion method. The Ag/SiO_2 nanocomposites were characterized by UV–vis spectra, transmission electron microscopy (TEM) and atom force microscopy (AFM). The antibacterial experiments demonstrated the nanoparticles had a high and long-lived antibacterial activity toward gram-positive and gram-negative bacteria.
In chapter 6, the mesoporous nanocomposites Ag/MCM-41 were prepared respectively by a one-route procedure and a two-route one. Structural analyses have showed that nanoscale silver particles uniformly distributed inner the holes and on the surface of MCM-41 matrix. High antibacterial activities toward gram-positive and gram-negative bacteria attributed to conjunct actions of Ag+ ion and silver nanoparticles.
In chapter 7, the mesoporous Ag/SBA-15 nanocomposites were prepared by a two-step procedure. The Ag/SBA-15 nanocomposites were systemically characterized by UV–vis spectra, transmission electron microscopy (TEM), atom force microscopy (AFM) and so on. The antibacterial activity of the Ag/SBA-15 nanocomposites was also studied. The results showed that the sample has high antibacterial activity toward gram-positive and gram-negative.
引文
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