Süslü Incilay, Ozaltin Nuran, Altinöz Sacide
Hacettepe University, Faculty of Pharmacy, Department of Analytical Chemistry, 06100 Sihhiye, Ankara, Turkey.
J AOAC Int. 2010 Mar-Apr;93(2):562-8.
The aim of this study was to develop a new, simple, rapid, and sensitive square-wave adsorptive stripping voltammetric method for the determination of candesartan cilexetil in bulk form and pharmaceutical formulations by complex formation with Cu(II). The experimental and instrumental parameters affecting the response of the candesartan cilexetil-Cu(II) complex were investigated and optimized. This method was based on electrochemical reduction of candesartan cilexetil-Cu(II) complex at a hanging mercury drop electrode in phosphate buffer at pH 3.0 containing CuCl2 x 2H2O. A well-defined reduction peak was observed at -325 mV with 30 s accumulation time and -150 mV accumulation potential versus an Ag/AgCl reference electrode in the proposed method. The developed voltammetric method was validated in terms of linearity, sensitivity, precision, accuracy, recovery, selectivity, robustness, and ruggedness. The linear calibration range was 0.50-1.77 microg/mL (r = 0.9972). The LOD and LOQ of this method were 0.10 and 0.50 microg/mL (n = 7), respectively. The developed method was fully validated and applied to the pharmaceutical formulations, including candesartan cilexetil.
本研究的目的是开发一种新的、简单、快速且灵敏的方波吸附溶出伏安法,通过与Cu(II)形成络合物来测定坎地沙坦酯的原料药和药物制剂。研究并优化了影响坎地沙坦酯-Cu(II)络合物响应的实验和仪器参数。该方法基于坎地沙坦酯-Cu(II)络合物在含CuCl2·2H2O的pH 3.0磷酸盐缓冲液中的悬汞滴电极上进行电化学还原。在所提出的方法中,与Ag/AgCl参比电极相比,在-325 mV处观察到一个明确的还原峰,积累时间为30 s,积累电位为-150 mV。所开发的伏安法在线性、灵敏度、精密度、准确度、回收率、选择性、稳健性和耐用性方面进行了验证。线性校准范围为0.50 - 1.77 μg/mL(r = 0.9972)。该方法的检测限和定量限分别为0.10和0.50 μg/mL(n = 7)。所开发的方法经过充分验证,并应用于包括坎地沙坦酯在内的药物制剂。