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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([BnMIM]PF6)复合修饰碳糊电极(nano-TiO2-[BnMIM]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-[BnMIM]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-[BnMIM]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5.0×10-5～1.0×10-3mol·L-1呈线性关系,检测限(S/N=3)为1.20×10-7mol·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-[BnMIM]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: To study the effect of Aceclofenac (AC) on the surface of carbon paste electrode with nano-TiO2 and ionic liquid 1-benzyl-3-methylimidazolium hexafluorophosphate ([BnMIM] PF6) nano-TiO2- [BnMIM] PF6 / CPE) on the electrochemical behavior and electrochemical kinetic properties of AC electrochemical quantitative determination of the established method. Methods: Cyclic voltammetry (CV), chronoamperometry (CA), chrono coulometry (CC), square wave voltammetry (SWV) and electrochemical impedance spectroscopy (EIS) were used. Results: The diffusion-controlled irreversible electrochemical oxidation of AC on nano-TiO2- [BnMIM] PF6 / CPE occurred. The kinetic parameters of AC reaction on nano-TiO2- [BnMIM] PF6 / CPE were measured. The peak current of AC oxidation peaked at a concentration of 5.0 × 10-5 ~ 1.0 × 10-3 mol·L-1 by SWV. The detection limit (S / N = 3) was 1.20 × 10-7 mol·L-1 . The method was applied to the electrochemical quantitative determination of aceclofenac tablets with the RSD between 1.9% and 3.0% and the recoveries of spiked samples between 98.6% and 103.7%. CONCLUSION: nano-TiO2- [BnMIM] PF6 / CPE can catalyze the electrochemical oxidation of AC. This method can be used for the electrochemical quantitative determination of aceclofenac in the market.