Sefuroksim Aksetil' in Voltametrik Davranışlarının İncelenmesi ve Elektroanalitik Yöntemlerle Farmasötik Preparatlardan Analizi

Abstract

In this thesis, square wave voltammetric (SWV) methods have been developed for the quantitative determination of cefuroxime axetil (CEFA) from pharmaceutical preparations. Electrochemical reduction and oxidation of the substance on hanging mercury drop electrode (HMDE) and modified glassy carbon electrode (M-GCE) were investigated by SWV methods. For the determination of CEFA, firstly, supporting electrolyte pH, type and concentration were determined, then reduction and oxidation conditions were optimized. For HMDE, well-defined peaks were obtained with a frequency of 40 Hz, potential increment of 5 mV, pulse amplitude of 35 mVand limit of detection (LOD), limit of quantification (LOQ) and linearity range were found 0.086 μg mL-1, 0.263 μg mL-1, 0.263-14.773 μg mL-1, respectively. For M-GCE, well-defined peaks were obtained with a frequency of 45 Hz, potential increment of 5 mV, pulse amplitude of 60 mV and LOD, LOQ and linearity range were found 2.705 μg mL-1, 8.197 μg mL-1, 8.197-45.454 μg mL-1, respectively. According to validation studies, the developed SWV methods were found as accurate, precise, specific, sensitive, repeatable and robust. The developed and validated SWV methods were applied to the determination of CEFA in pharmaceutical formulations. The results were compared with those obtained by a published ultraviolet spectroscopic method and no difference was found statistically. In addition, electrochemical behaviours of CEFA were investigated on both HMDE and M-GCE. For this purpose, current type and reversibility of electrode reaction were investigated by using cyclic voltammetry (CV), chronoamperometry (CA), chronocoulometry (CC). Besides the calculating diffusion coefficient (D), rate constant of chemical reaction (k) and rate constant of electron transfer (kf), the reduction and oxidation mechanisms were also proposed