纳米金—声致发光分析方法研究

发布时间：2018-03-11 00:05

本文选题：纳米金　切入点：声致发光　出处：《陕西师范大学》2015年硕士论文　论文类型：学位论文

【摘要】：纳米金(AuNPs)具有独特的物理、光学、催化性质和良好的生物相容性,在医学、生物、化学等领域受到了广泛研究和应用。AuNPs在分析化学中的应用主要是基于其光学性质尺寸依赖效应,研究对分析物高灵敏度、选择性检测的分析方法,包括比色法、荧光分析法、电化学分析法、化学发光法。声致发光(SL)是液体中超声空化作用引起的光辐射效应。对SL研究和应用涉及物理、化学、生物、医学等领域。SL作为一类新的光谱分析方法,在分析化学中应用始于20世纪八十年代末。尽管到目前为止SL在分析化学中的研究已有近三十年历史,但是与SL其它领域基础理论研究相比,SL分析方法研究仍然很少。本论文旨在研究AuNPs在SL中分析方法,由综述和研究报告两部分组成。综述部分简要介绍了纳米金研究史,合成方法与基本性质,以及纳米金在医学、生物学中主要应用,重点讲述了纳米金在分析化学领域已建立的分析方法和应用研究。研究报告部分,讲述AuNPs-SL分析方法研究和AuNPs-声致化学发光(SCL)分析,具体内容：一、纳米金一声致发光检测三聚氰胺利用纳米材料识别分析物,结合纳米金和声致发光,建立了一种灵敏、简单的检测奶制品中三聚氰胺SL法。水的SL作为内置光源,13 nm分散态金纳米粒子吸收520 nm处水SL。三聚氰胺通过配体交换和氢键作用团聚纳米金,使纳米金表面等离子体吸收峰红移,导致520 nm处水声致发光恢复。通过测量520 nm处水声致发光信号变化实现对三聚氰胺定量分析。实验考查了超声时间和时间间隔、纳米金用量、纳米金与三聚氰胺作用时间、检测液体积对SL影响。最优实验条件下,SL信号与三聚氰胺浓度10nM-240nM呈良好线性关系,线性方程为△I= 25.5 CMelamine(10 nM)+125.9 (R2=0.991),检出限3 nM。对浓度10 nM的三聚氰胺溶液进行了21次的平行测定,相对标准偏差为2.3%,说明SL法重现性很好。用SL检测牛奶样品中三聚氰胺,实验结果与高效液相色谱法一致。F、t检验数据分析表明本方法具有很好的准确性。二、纳米金—鲁米诺声致化学发光分析实验发现,金纳米粒子存在时,过氧化氢能够增强鲁米诺SCL。进一步实验证明,纳米金—鲁米诺—过氧化氢SCL随过氧化氢浓度增加而增大,基于此现象建立了检测过氧化氢的SCL法。实验考查了对纳米金—鲁米诺—过氧化氢SCL信号随时间变化和影响SCL的因素(鲁米诺浓度、纳米金用量、纳米金超声分散时间)。将柠檬酸和鲁米诺还原制备的纳米金对过氧化氢检测灵敏度差异进行了简单的比较。通过SCL反应前后UV/Vis和TEM表征,对纳米金—鲁米诺—过氧化氢SCL机理进行了探讨。此外,还讨论了纳米金—鲁米诺SCL体系其它分析应用。
[Abstract]:Nano au au NPs) have unique physical, optical, catalytic properties and good biocompatibility in medicine, biology, The application of AuNPs in analytical chemistry has been extensively studied and applied in the field of chemistry, which is mainly based on the size dependence effect of optical properties. The analytical methods of high sensitivity and selectivity to the analyte, including colorimetric method, fluorescence analysis method, are studied. Electrochemical analysis, chemiluminescence method, sonoluminescence (SLL) is the light radiation effect caused by ultrasonic cavitation in liquid. The research and application of SL involves physics, chemistry, biology, medicine and other fields as a new kind of spectral analysis method. Its application in analytical chemistry began at the end of 1980s. Although SL has been studied in analytical chemistry for nearly 30 years, However, compared with other basic theoretical studies in SL, there are few researches on SL analytical methods. This thesis aims to study the analytical methods of AuNPs in SL, which consists of two parts: a review and a research report. The review section briefly introduces the history of gold nanocrystalline analysis. The synthetic methods and basic properties, as well as the main applications of nanocrystalline gold in medicine and biology are described. The analytical methods and applied research in the field of analytical chemistry are described in detail. This paper describes the research of AuNPs-SL analysis method and AuNPs- sonoluminescence analysis. The main contents are as follows: first, the detection of melamine by nanocrystalline sonoluminescence using nanomaterial to identify the analyte, combined with nano-gold and sonoluminescence, to establish a kind of sensitivity. A simple method for the detection of melamine SL in dairy products. SL of water is used as a built-in light source for 13 nm dispersed gold nanoparticles to absorb water SLL at 520 nm. Melamine agglomerates gold nanoparticles by ligand exchange and hydrogen bonding. The absorption peak of nanocrystalline gold surface plasma is redshift, resulting in the recovery of underwater sonoluminescence at 520 nm. The quantitative analysis of melamine is realized by measuring the variation of sonoluminescence signal at 520 nm. The ultrasonic time and time interval are investigated experimentally. The amount of nano-gold, the reaction time of nano-gold and melamine, and the volume of detection liquid had a good linear relationship with the concentration of melamine 10nM-240nM under the optimal experimental conditions. The linear equation is I = 25.5 CMelamine(10 NM) 125.9 CMelamine(10 NM). The detection limit is 3 nm. 21 times parallel determination of melamine solution with 10 nm concentration has been carried out, and the relative standard deviation is 2.3. The result shows that SL method has good reproducibility, and can be used to detect melamine in milk samples. The experimental results are consistent with the results of HPLC. FUT test data analysis shows that the method has good accuracy. Secondly, the results of nanocrystalline gold luminol sonoluminescence analysis show that gold nanoparticles exist in the presence of gold nanoparticles. Hydrogen peroxide can enhance Luminol SCL. further experiments show that the SCL of nanocrystalline gold-Lumino-hydrogen peroxide increases with the increase of hydrogen peroxide concentration. Based on this phenomenon, a SCL method for the detection of hydrogen peroxide was established. The changes of SCL signal of nanocrystalline-Lumino-hydrogen peroxide over time and the factors affecting SCL (concentration of Lumino, dosage of nanometer gold) were investigated. Nano-gold ultrasonic dispersion time. The sensitivity of nanocrystalline gold prepared by reduction of citric acid and Lumino to hydrogen peroxide was compared. The results were characterized by UV/Vis and TEM before and after SCL reaction. The mechanism of nanocrystalline gold-Lumino-hydrogen peroxide SCL was discussed. In addition, other analytical applications of nanocrystalline-Lumino SCL system were also discussed.
【学位授予单位】：陕西师范大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：O657.3;TB383.1

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