水环境中氧氟沙星的电分析检测研究

发布时间：2018-07-26 17:08

【摘要】：氧氟沙星(OFL)是一种典型的喹诺酮类广谱抗生素,在医用和兽用方面使用广泛。近年来,在各类水环境介质中被频繁检出,受到越来越多的关注。因此制备出简便、快速、灵敏的电化学传感器来实现对水环境中OFL的实时原位检测有着重要的作用及意义。本文运用两种电极修饰手段,通过电化学方法,旨在构建水环境中氧氟沙星的不同电化学检测方法。取得的主要成果如下:1、利用石墨烯(Gr)和金属铂纳米粒子(PtNPs)复合材料修饰玻碳电极,成功地制备成PtNPs/Gr/GCE电极。辅以扫描电子显微镜(SEM)、原子力显微镜(AFM)和能谱仪(EDS)表征修饰电极的界面性质。同时,一些实验测试参数,如石墨烯浓度、电解质pH、扫速等在本文中均作了讨论和优化。实验结果表明,在最佳优化条件下,该传感器对OFL的浓度响应范围为0.75?10-6-2.5?10-4mol L-1,检出限为0.75?10-6 mol L-1。传感器应用于地下水和自来水中OFL的测定,回收率范围在93.90%-102.34%之间,相对标准偏差(R.S.D.)均小于2.83%。2、利用激光修饰玻碳电极,构建了一种新颖的电化学传感器。通过增加电极表面有效面积及氧官能团种类和数量,以增强电极表面的电化学活性。并对水环境的OFL进行电分析检测。通过对激光修饰电极界面的SEM、X射线光电子能谱分析(XPS)、AFM表征,探讨了电极表面活性提高的机理。在实验参数最优化的条件下,该修饰电极对OFL浓度的检出线性响应范围为2.5?10-7-2?10-4mol L-1,检出限为7.5?10-8mol L-1,将该传感器应用于地下水和自来水中OFL的测定,回收率范围都在94%-108%之间,R.S.D.均小于4.80%。3、本文分别利用纳米材料和激光制备了两种修饰电极,这两种电化学传感器检测OFL均具有较宽的线性范围和较低的检出限,且具有良好的稳定性和重现性等特点。此外,在全部检测过程中,体系无需驱O2,表明这两种电化学检测方法用于实际水环境中OFL的原位在线检测,具有较强的可行性。
[Abstract]:Ofloxacin (OFL) is a typical wide spectrum antibiotic of quinolones. It is widely used in medical and animal applications. In recent years, more and more attention has been made in various water environmental media. Therefore, the preparation of a simple, rapid and sensitive electrochemical sensor is important to realize real-time in situ detection of OFL in water environment. The purpose of this paper is to construct the different electrochemical detection methods of ofloxacin in water environment by means of two kinds of electrode modification methods. The main achievements are as follows: 1, using graphene (Gr) and metal platinum nanoparticles (PtNPs) composite materials to modify the glassy carbon electrode and successfully prepare the PtNPs/Gr/GCE electrode. Scanning electron microscopy (SEM), atomic force microscopy (AFM) and energy spectrometer (EDS) are used to characterize the interfacial properties of modified electrodes. At the same time, some experimental parameters, such as graphene concentration, electrolyte pH, and scanning speed, are discussed and optimized in this paper. The experimental results show that the sensor's concentration response to OFL is 0.7 under the optimum optimization conditions. 5? 10-6-2.5? 10-4mol L-1, the detection limit of 0.75? 10-6 mol L-1. sensor is applied to the determination of OFL in groundwater and tap water. The recovery rate is between 93.90%-102.34% and the relative standard deviation (R.S.D.) is less than 2.83%.2. A novel electrochemical sensor is constructed by laser modified glassy carbon electrode. The effective surface of the electrode surface is increased by increasing the effective surface of the electrode surface. The type and quantity of oxygen functional groups were accumulated and the electrochemical activity of the electrode surface was enhanced. The OFL of the water environment was detected by electric analysis. The mechanism of improving the surface activity of the electrode was discussed by SEM, X ray photoelectron spectroscopy (XPS) and AFM. The modified electrode was optimized under the condition of the optimum experimental parameters. The linear response range of OFL concentration was 2.5? 10-7-2? 10-4mol L-1, and the detection limit was 7.5? 10-8mol L-1. The sensor was applied to the determination of OFL in groundwater and tap water. The recovery rate was between 94%-108% and R.S.D. less than 4.80%.3. In this paper, two kinds of modified electrodes were prepared by using nanoscale material and laser. These two kinds of electrochemical transmission were carried out in this paper. The sensilla detection OFL has a wide linear range and a lower detection limit, and has good stability and reproducibility. In addition, the system does not need to drive O2 during the whole detection process, indicating that these two electrochemical detection methods are applied to the in-situ on-line detection of OFL in the actual water environment, which has a strong feasibility.
【学位授予单位】：中国地质大学(北京)
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：X832;O657.1

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