醋氯芬酸在nano-TiO₂/PF₆修饰碳糊电极上的电催化氧化及电分析方法

目的: 研究了醋氯芬酸(Aceclofenac,AC)在纳米二氧化钛(nano-TiO₂)与离子液体1-苄基-3-甲基咪唑六氟磷酸盐( PF₆)复合修饰碳糊电极(nano-TiO₂- PF₆/CPE)上的电化学行为和电化学动力学性质,建立了AC电化学定量测定方法。 方法: 循环伏安法(CV),计时电流法(CA),计时库仑法(CC),方波伏安法(SWV)以及电化学交流阻抗法(EIS)。 结果: 在nano-TiO₂- PF₆/CPE上AC发生了受扩散控制的不可逆电化学氧化过程。测得AC在nano-TiO₂- PF₆/CPE上的电极反应过程动力学参数。用SWV法测得AC氧化峰电流与其浓度在5.0×10 ^-5~1.0×10 ^-3 mol·L^-1呈线性关系,检测限(S/N=3)为1.20×10 ^-7 mol·L^-1。采用本方法对市售醋氯芬酸片进行了电化学定量测定,RSD在1.9%~3.0%之间,加标回收率在98.6%~103.7%之间。 结论: nano-TiO₂- PF₆/CPE 对AC电化学氧化具有良好的催化作用,该方法可用于市售醋氯芬酸含量的电化学定量测定。

Objective: Studied the electrochemical behaviors and electrochemical kinetic of Aceclofenac (AC) at nano-TiO₂ and 1-Benzyl-3-Methylimidazole hexafluorophosphate ( PF₆) modified carbon paste electrode (CPE).At the same time,one electrochemical quantitative determination had been established. Methods: Cyclic Voltammetry (CV),Chronocoulometry (CC),Chronoamperometry (CA),Electrochemical Impedance Spectrum (EIS) and Square Wave Voltammetry (SWV). Results: Electrochemical experimental results show that AC electrochemical behavior in 0.10 mol·L^-1PBS exhibits an irreversible electrochemical redox process at nano-TiO₂- PF₆/ CPE.The electrochemical kinetics of Aceclofenac (AC) at nano-TiO₂- PF₆/ CPE were measured.The oxidation peak current of AC versus its concentration have a good linear relationship in the concentration range of 5.0×10 ^-5-1.0×10 ^-3 mol·L^-1 and the detection limit of 1.20×10 ^-7 mol·L^-1 by Square wave voltammetry (SWV) response.The quantitative determination of Aceclofenac (AC) content was investigated,the relative standard deviation is between 1.9%-3.0% and the recoverage is in the range of 98.56%-103.7%. Conclusion: The experimental result indicated that nano-TiO₂- PF₆/CPE could catalyze the oxidation of AC well.Furthermore,this method can be applied in the test of Aceclofenac content with simple manipulation.