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氢氧化镍纳米颗粒-还原氧化石墨烯纳米片薄膜:逐层电化学制备、表征及利福平传感应用。

Nickel hydroxide nanoparticles-reduced graphene oxide nanosheets film: layer-by-layer electrochemical preparation, characterization and rifampicin sensory application.

作者信息

Rastgar Shokoufeh, Shahrokhian Saeed

机构信息

Department of Chemistry, Sharif University of Technology, Tehran 11155-9516, Iran.

Department of Chemistry, Sharif University of Technology, Tehran 11155-9516, Iran; Institute for Nanoscience and Technology, Sharif University of Technology, Tehran, Iran.

出版信息

Talanta. 2014 Feb;119:156-63. doi: 10.1016/j.talanta.2013.10.047. Epub 2013 Nov 7.

DOI:10.1016/j.talanta.2013.10.047
PMID:24401398
Abstract

Electrochemical deposition, as a well-controlled synthesis procedure, has been used for subsequently layer-by-layer preparation of nickel hydroxide nanoparticle-reduced graphene oxide nanosheets (Ni(OH)2-RGO) on a graphene oxide (GO) film pre-cast on a glassy carbon electrode surface. The surface morphology and nature of the nano-hybrid film (Ni(OH)2-RGO) was thoroughly characterized by scanning electron and atomic force microscopy, spectroscopy and electrochemical techniques. The modified electrode appeared as an effective electro-catalytic model for analysis of rifampicin (RIF) by using linear sweep voltammetry (LSV). The prepared modified electrode exhibited a distinctly higher activity for electro-oxidation of RIF than either GO, RGO nanosheets or Ni(OH)2 nanoparticles. Enhancement of peak currents is ascribed to the fast heterogeneous electron transfer kinetics that arise from the synergistic coupling between the excellent properties of RGO nanosheets (such as high density of edge plane sites, subtle electronic characteristics and attractive π-π interaction) and unique properties of metal nanoparticles. Under the optimized analysis conditions, the modified electrode showed two oxidation processes for rifampicin at potentials about 0.08 V (peak I) and 0.69 V (peak II) in buffer solution of pH 7.0 with a wide linear dynamic range of 0.006-10.0 µmol L(-1) and 0.04-10 µmol L(-1) with a detection limit of 4.16 nmol L(-1) and 2.34 nmol L(-1) considering peaks I and II as an analytical signal, respectively. The results proved the efficacy of the fabricated modified electrode for simple, low cost and highly sensitive medicine sensor well suited for the accurate determinations of trace amounts of rifampicin in the pharmaceutical and clinical preparations.

摘要

电化学沉积作为一种可控的合成方法,已被用于在预先浇铸在玻碳电极表面的氧化石墨烯(GO)薄膜上逐层制备氢氧化镍纳米颗粒还原氧化石墨烯纳米片(Ni(OH)₂-RGO)。通过扫描电子显微镜、原子力显微镜、光谱学和电化学技术对纳米复合薄膜(Ni(OH)₂-RGO)的表面形态和性质进行了全面表征。修饰电极通过线性扫描伏安法(LSV)成为分析利福平(RIF)的有效电催化模型。制备的修饰电极对RIF的电氧化表现出明显高于GO、RGO纳米片或Ni(OH)₂纳米颗粒的活性。峰电流的增强归因于快速的异相电子转移动力学,这是由RGO纳米片的优异性能(如高密度的边缘平面位点、微妙的电子特性和有吸引力的π-π相互作用)与金属纳米颗粒的独特性能之间的协同耦合产生的。在优化的分析条件下,修饰电极在pH 7.0的缓冲溶液中对利福平显示出两个氧化过程,电位分别约为0.08 V(峰I)和0.69 V(峰II),线性动态范围宽,分别为0.006 - 10.0 μmol L⁻¹和0.04 - 10 μmol L⁻¹,以峰I和峰II作为分析信号时检测限分别为4.16 nmol L⁻¹和2.34 nmol L⁻¹。结果证明了所制备的修饰电极作为简单、低成本且高灵敏度药物传感器的有效性,非常适合准确测定药物制剂和临床制剂中的痕量利福平。

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