三乙醇胺功能化金纳米粒子和二氧化硅纳米粒子的分析特性研究
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摘要
纳米材料具有不同于宏观物质的性质,是现代材料科学研究的热点之一。纳米材料的功能化是纳米材料研究和应用的基础。本学位论文首先综述了金纳米粒子的性质、制备方法、在分析化学中的应用及功能化金纳米粒子的意义和方法。在三乙醇胺可以通过静电作用修饰在纳米粒子的表面的基础上,建立了三乙醇胺功能化金纳米粒子和二氧化硅纳米粒子测定金属离子的分析方法,具体工作如下：
一、三乙醇胺功能化金纳米粒子比色分析法的研究。
半胱氨酸和巯基乙酸可以通过巯基与金纳米粒子形成Au-S键,被固定在金纳米粒子的表面。钙离子与半胱氨酸分子中的氨基和羧基的配位作用,可以迅速引起功能化的金纳米粒子发生团聚。同时,当三乙醇胺通过静电作用被进一步修饰到功能化金纳米粒子表面,可以有效金降低金纳米粒子表面的静电斥力,从而提高了金纳米粒子比色分析方法的灵敏度。透射电子显微镜、紫外可见吸收实验和电泳实验等用于该比色分析方法实现对钙离子和镁离子的测定。在最佳实验条件下,半胱氨酸-巯基乙酸-三乙醇胺修饰的金纳米粒子对钙离子和镁离子的响应具有良好的选择性和较高的灵敏度,对钙离子测定的检出限为3.0×10-7 mol·L-1。在1.0×10-6 mol·L-1到1.4×10-5 mol·L-1范围内,金纳米粒子的吸光度与钙镁离子的浓度呈线性关系。
二、基于三乙醇胺功能化联钌吡啶-二氧化硅纳米粒子构建铜离子传感器的研究。
研究发现三乙醇胺可通过静电作用吸附于联钌吡啶-二氧化硅纳米粒子表面,形成三乙醇胺功能化的二氧化硅荧光纳米粒子。在此研究基础上,基于三乙醇胺与铜离子的配位效应,以及铜离子对联钌吡啶荧光的猝灭作用,构建了铜离子纳米粒子传感器。在优化的试验条件下,该传感器对铜离子测定的检出限为2.0×10-6 mol·L-1,响应线性范围为6.0×10-6 mol·L-1到1.0×10-4 mol·L-1。
Nowadays, nanomaterials have been the focus of modern scientific due to the unique physical properties. Functional nanomaterials are the basis of the study and application of nanomaterials. This thesis reviews the nature of gold nanoparticles, preparation methods, application in analytical chemistry and significance and methods of functionalization of gold nanoparticles. Analytical method for metal ions was established based on triethanolamine functional gold nanoparticles and silica nanoparticles. The thesis includes the following parts:
1. Colorimetric method based on triethanolamine functional gold nanoparticles.
It was found that, after cysteine and thioglycolic acid were immobilized on the surface of gold nanoparticles with the thiol-Au chemistry, calcium ion could rapidly induce aggregation of the functional gold nanoparticles based on complex effect of calcium ion with amino and carboxyl groups in the immobilized cysteine molecules. At the same time, it was also found that triethanolamine could obviously enhance the sensitivity of calcium ion based on decreasing the electrostatic repulsion force between the interparticle gold nanoparticles. Thereafter, the Transmission Electron Microscopy, electrophoresis technique and absorption spectrum method, were used to investigate the sensing mechanism of the functional gold part les for calcium ion. Under the optimum experiment condition, the cysteine-thioglycolic acid-triethanolamine modified gold nanoparticles were highly sensitive (the detection limit was 3.0×10-7 mol·L-1) and selective toward calcium and magnesium ions, with a linear detection range from 1.0×10-6 mol·L-1 to 1.4×10-5 mol·L-1. Based on these findings, a rapid, simple and selective colorimetric method for assaying the hardness in tap water was developed.
2. The fabrication of Copper Ions fluorescence nanosensor with Triethanolamine Functionalizing Ru(bpy)32+-doped Silica Nanoparticles.
It was found that triethanolamine could be adsorbed on the surface of Ru(bpy)32+-doped SiO2 nanoparticles based on electrostatic interaction of triethanolamine with silica nanoparticles. Then, based on the complex effect between copper ions and triethanolamine as well as the quenching effect of copper ions for doped state Ru(bpy)32+, a fluorescence nanosensor for copper ions was developed. Under the optimum experiment condition, the detection limit of the nanosensor for copper ions was 2.0×10-6 mol·L-1 and the response dynamic range was from 6.0×10-6 mol·L-1 to 1.0×10-4 mol·L-1.
一、三乙醇胺功能化金纳米粒子比色分析法的研究。
半胱氨酸和巯基乙酸可以通过巯基与金纳米粒子形成Au-S键,被固定在金纳米粒子的表面。钙离子与半胱氨酸分子中的氨基和羧基的配位作用,可以迅速引起功能化的金纳米粒子发生团聚。同时,当三乙醇胺通过静电作用被进一步修饰到功能化金纳米粒子表面,可以有效金降低金纳米粒子表面的静电斥力,从而提高了金纳米粒子比色分析方法的灵敏度。透射电子显微镜、紫外可见吸收实验和电泳实验等用于该比色分析方法实现对钙离子和镁离子的测定。在最佳实验条件下,半胱氨酸-巯基乙酸-三乙醇胺修饰的金纳米粒子对钙离子和镁离子的响应具有良好的选择性和较高的灵敏度,对钙离子测定的检出限为3.0×10-7 mol·L-1。在1.0×10-6 mol·L-1到1.4×10-5 mol·L-1范围内,金纳米粒子的吸光度与钙镁离子的浓度呈线性关系。
二、基于三乙醇胺功能化联钌吡啶-二氧化硅纳米粒子构建铜离子传感器的研究。
研究发现三乙醇胺可通过静电作用吸附于联钌吡啶-二氧化硅纳米粒子表面,形成三乙醇胺功能化的二氧化硅荧光纳米粒子。在此研究基础上,基于三乙醇胺与铜离子的配位效应,以及铜离子对联钌吡啶荧光的猝灭作用,构建了铜离子纳米粒子传感器。在优化的试验条件下,该传感器对铜离子测定的检出限为2.0×10-6 mol·L-1,响应线性范围为6.0×10-6 mol·L-1到1.0×10-4 mol·L-1。
Nowadays, nanomaterials have been the focus of modern scientific due to the unique physical properties. Functional nanomaterials are the basis of the study and application of nanomaterials. This thesis reviews the nature of gold nanoparticles, preparation methods, application in analytical chemistry and significance and methods of functionalization of gold nanoparticles. Analytical method for metal ions was established based on triethanolamine functional gold nanoparticles and silica nanoparticles. The thesis includes the following parts:
1. Colorimetric method based on triethanolamine functional gold nanoparticles.
It was found that, after cysteine and thioglycolic acid were immobilized on the surface of gold nanoparticles with the thiol-Au chemistry, calcium ion could rapidly induce aggregation of the functional gold nanoparticles based on complex effect of calcium ion with amino and carboxyl groups in the immobilized cysteine molecules. At the same time, it was also found that triethanolamine could obviously enhance the sensitivity of calcium ion based on decreasing the electrostatic repulsion force between the interparticle gold nanoparticles. Thereafter, the Transmission Electron Microscopy, electrophoresis technique and absorption spectrum method, were used to investigate the sensing mechanism of the functional gold part les for calcium ion. Under the optimum experiment condition, the cysteine-thioglycolic acid-triethanolamine modified gold nanoparticles were highly sensitive (the detection limit was 3.0×10-7 mol·L-1) and selective toward calcium and magnesium ions, with a linear detection range from 1.0×10-6 mol·L-1 to 1.4×10-5 mol·L-1. Based on these findings, a rapid, simple and selective colorimetric method for assaying the hardness in tap water was developed.
2. The fabrication of Copper Ions fluorescence nanosensor with Triethanolamine Functionalizing Ru(bpy)32+-doped Silica Nanoparticles.
It was found that triethanolamine could be adsorbed on the surface of Ru(bpy)32+-doped SiO2 nanoparticles based on electrostatic interaction of triethanolamine with silica nanoparticles. Then, based on the complex effect between copper ions and triethanolamine as well as the quenching effect of copper ions for doped state Ru(bpy)32+, a fluorescence nanosensor for copper ions was developed. Under the optimum experiment condition, the detection limit of the nanosensor for copper ions was 2.0×10-6 mol·L-1 and the response dynamic range was from 6.0×10-6 mol·L-1 to 1.0×10-4 mol·L-1.
引文
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