Acta Chim Slov. 2020 Sep;67(3):729-738.
In this study, the nano-sepiolite modified carbon paste electrode (CCPE) was prepared for the determination of ketoconazole (KC). The effects of pH, the proportion of the electrode modifier, deposition potential, and deposition time were investigated. Ketoconazole shows one irreversible oxidation peak at about the potential value of 0.6-0.7 V at different pH values. CV studies show that the modified electrode performed a catalytic effect on the peak signal of KC compared to the bare electrode. This catalytic behavior of CCPE was used for the development of a sensitive detection method. The impact of pH and scan rates on the anodic peak potentials and currents were examined, and the scan rate results show that the oxidation behavior of KC was controlled by the adsorption process at the CCPE surface. Therefore, adsorptive stripping differential pulse voltammetry (AdsDPV) and adsorptive stripping square wave voltammetry (AdsSWV) methods were developed for KC analysis. The two different linear ranges were obtained as (0.1?1.0) nM and (3.0?10.0) nM for AdsDPV, and (0.1-10.0) nM and (3.0-10.0) nM for AdsSWV, respectively. The detection (LOD) and quantification (LOQ) limits were found to be 0.017 nM and 0.056 nM for AdsDPV and 0.025 nM and 0.083 nM for AdsSWV, respectively. Besides, the proposed new sensor has obtained very high recovery values in the analysis of KC in the pharmaceutical shampoo.
在这项研究中，制备了纳米海泡石修饰碳糊电极（CCPE）用于测定酮康唑（KC）。考察了 pH 值、电极修饰剂的比例、沉积电位和沉积时间的影响。在不同 pH 值下，酮康唑在约 0.6-0.7 V 的电位值处显示出一个不可逆的氧化峰。CV 研究表明，与裸电极相比，修饰电极对 KC 的峰信号表现出催化作用。CCPE 的这种催化行为被用于开发一种灵敏的检测方法。考察了 pH 值和扫描速率对阳极峰电位和电流的影响，扫描速率结果表明 KC 的氧化行为受 CCPE 表面的吸附过程控制。因此，开发了用于 KC 分析的吸附溶出差分脉冲伏安法（AdsDPV）和吸附溶出方波伏安法（AdsSWV）。对于 AdsDPV，得到了两个不同的线性范围，分别为（0.1?1.0）nM 和（3.0?10.0）nM，对于 AdsSWV，分别为（0.1-10.0）nM 和（3.0-10.0）nM。发现 AdsDPV 的检测限（LOD）和定量限（LOQ）分别为 0.017 nM 和 0.056 nM，AdsSWV 的检测限（LOD）和定量限（LOQ）分别为 0.025 nM 和 0.083 nM。此外，在药物香波中分析 KC 时，所提出的新传感器获得了非常高的回收率值。
