新型Fe_3O_4纳米颗粒修饰玻碳电极对头孢噻肟钠的电催化还原及其测定  

The Electrocatalytic Reduction and Determination of Cefotaxime Sodium by a Glass Carbon Electrode Modified with Nano-Fe_3O_4 Particles

作　　者：王明艳[1,2] 杨俊[1] 周琴[1] 陈龙[1] 陶智鹏 

机构地区：[1]淮海工学院化学工程学院,连云港222005 [2]南京理工大学材料化学实验室,南京210094

出　　处：《应用化学》2012年第3期346-352,共7页Chinese Journal of Applied Chemistry

基　　金：国家自然科学基金(50873042);江苏省海洋资源开发研究院科技开放基金(JSIMR09B05);江苏省海洋生物技术重点建设实验室开放基金(2010HS11)资助项目

摘　　要：采用滴涂法将Fe3O4磁性纳米颗粒修饰在玻碳电极上,制得新型纳米Fe3O4修饰电极(Fe3O4-np/GC电极)。X射线衍射光谱表明,纳米Fe3O4为面心立方尖晶石结构,透射电子显微镜表明,纳米Fe3O4粒径15～20 nm的微球结构。采用扫描电子显微镜和交流阻抗法(EIS)对修饰电极表面进行了表征,发现纳米Fe3O4在电极表面形成了均匀的修饰膜。采用循环伏安法(CV)、微分脉冲伏安法(DPV)研究了头孢噻肟钠(CS)在修饰电极上的电化学行为及动力学性质,结果表明,CS在Fe3O4-np/GC电极上有敏锐的催化还原峰,且CS的还原峰电流与其浓度在7.0×10-8～1×10-6和1×10-6～4.5×10-5mol/L范围内呈线性关系;检出限达到5.0×10-8mol/L。该方法可用于市售头孢噻肟钠针剂中CS含量的测定,加标回收率达到96.6%～102.7%。A novel Fe3O4 nanoparticles modified glassy carbon electrode （Fe3Q-np/GC electrode） was fabricated via a dropwise-coating method. The XRD pattern indicated that the Fe3O4 nanoparticles have pure cubic phase spinel structure, and the TEM image showed that the Fe3O4 nanoparticles are tiny spherical particles with mean size of 15 - 20 nm. The microstructure and electrochemical behavior of the modified electrode were investigated by scanning electron microscope （SEM） and electrochemical impedance spectrum （EIS）. The electrochemical behaviors and kinetic parameters of cefotaxime sodium （CS） on Fe304-np/GC electrode were investigated by cyclic voltammetry （CV） and differential pulse voltammetry （DPV）. The experimental results showed that the reduction peak current of CS increased significantly at modified electrode in comparison with that at GC electrode. In B-R buffer solution, the reduction peak currents are proportional to the concentrations of CS over the range from 7.0 ×10^-8 to 1× 10^-6 and 1×10^-6 to 4. 5×10^-5 mol/L, respectively, and the limit of detection is 5.0×10^-8 mol/L. This method was applied in the determination of CS in four kinds of commercial injection samples and the recovery varies from 96. 6% to 102.7%.

关 键 词：修饰电极 FE3O4纳米颗粒 头孢噻肟钠 电催化 

分 类 号：O657[理学—分析化学]