發(fā)布時間：2018-07-26 17:08

【摘要】：氧氟沙星(OFL)是一種典型的喹諾酮類廣譜抗生素,在醫(yī)用和獸用方面使用廣泛。近年來,在各類水環(huán)境介質(zhì)中被頻繁檢出,受到越來越多的關(guān)注。因此制備出簡便、快速、靈敏的電化學(xué)傳感器來實現(xiàn)對水環(huán)境中OFL的實時原位檢測有著重要的作用及意義。本文運用兩種電極修飾手段,通過電化學(xué)方法,旨在構(gòu)建水環(huán)境中氧氟沙星的不同電化學(xué)檢測方法。取得的主要成果如下:1、利用石墨烯(Gr)和金屬鉑納米粒子(PtNPs)復(fù)合材料修飾玻碳電極,成功地制備成PtNPs/Gr/GCE電極。輔以掃描電子顯微鏡(SEM)、原子力顯微鏡(AFM)和能譜儀(EDS)表征修飾電極的界面性質(zhì)。同時,一些實驗測試參數(shù),如石墨烯濃度、電解質(zhì)pH、掃速等在本文中均作了討論和優(yōu)化。實驗結(jié)果表明,在最佳優(yōu)化條件下,該傳感器對OFL的濃度響應(yīng)范圍為0.75?10-6-2.5?10-4mol L-1,檢出限為0.75?10-6 mol L-1。傳感器應(yīng)用于地下水和自來水中OFL的測定,回收率范圍在93.90%-102.34%之間,相對標準偏差(R.S.D.)均小于2.83%。2、利用激光修飾玻碳電極,構(gòu)建了一種新穎的電化學(xué)傳感器。通過增加電極表面有效面積及氧官能團種類和數(shù)量,以增強電極表面的電化學(xué)活性。并對水環(huán)境的OFL進行電分析檢測。通過對激光修飾電極界面的SEM、X射線光電子能譜分析(XPS)、AFM表征,探討了電極表面活性提高的機理。在實驗參數(shù)最優(yōu)化的條件下,該修飾電極對OFL濃度的檢出線性響應(yīng)范圍為2.5?10-7-2?10-4mol L-1,檢出限為7.5?10-8mol L-1,將該傳感器應(yīng)用于地下水和自來水中OFL的測定,回收率范圍都在94%-108%之間,R.S.D.均小于4.80%。3、本文分別利用納米材料和激光制備了兩種修飾電極,這兩種電化學(xué)傳感器檢測OFL均具有較寬的線性范圍和較低的檢出限,且具有良好的穩(wěn)定性和重現(xiàn)性等特點。此外,在全部檢測過程中,體系無需驅(qū)O2,表明這兩種電化學(xué)檢測方法用于實際水環(huán)境中OFL的原位在線檢測,具有較強的可行性。
[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.
【學(xué)位授予單位】：中國地質(zhì)大學(xué)(北京)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：X832;O657.1

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