Al-Ghamdi Ali F, Hefnawy Mohamed M, Al-Majed Abdulrahman A, Belal Fatallah F
Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, P,O, Box 2457, Riyadh 11451, Saudi Arabia.
Chem Cent J. 2012 Feb 21;6:15. doi: 10.1186/1752-153X-6-15.
A validated simple, rapid, sensitive and specific square-wave voltammetric technique is described for the determination of acebutolol (AC) following its accumulation onto a hanging mercury drop electrode in a Britton-Robinson universal buffer of pH 7.5. The optimal procedural conditions were: accumulation potential Eacc = - 0.8 V versus Ag/AgCl/KCl, accumulation duration tacc = 30 s, pulse-amplitude = 70 mV, scan rate = 100 mV/s, frequency = 30 Hz, surface area of the working electrode = 0.6 mm2 and the convection rate = 2000 rpm. Under these optimized conditions, the adsorptive stripping voltammetry (AdSV) peak current was proportional over the concentration range 5 × 10-7 - 6 × 10-6 M (r = 0.999). Recoveries for acebutolol from human plasma and urine were in the range 97-103% and 96-104% respectively. The method proved to be precise (intra-day precision expressed as %RSD in human plasma ranged from 2.9 - 3.2% and inter-day precision expressed as %RSD ranged from 3.4 - 3.8%) and accurate (intra-day accuracies expressed as % error in human urine ranged from -3.3 - 2.8% and inter-day accuracies ranged from -3.3 - 1.7%). The limit of quantitation (LOQ) and limit of detection (LOD) for acebutolol were 1.7 × 10-7 and 5 × 10-7 M, respectively. Possible interferences by substances usually present in the pharmaceutical formulations were investigated with a mean recovery of 101.6 ± 0.64%. Results of the developed square-wave adsorptive stripping voltammetry (SW-AdSV) method were comparable with those obtained by reference analytical method.
描述了一种经过验证的简单、快速、灵敏且特异的方波伏安法，用于在pH 7.5的Britton-Robinson通用缓冲液中，将醋丁洛尔（AC）富集到悬汞滴电极上后对其进行测定。最佳实验条件为：富集电位Eacc = -0.8 V（相对于Ag/AgCl/KCl），富集时间tacc = 30 s，脉冲幅度 = 70 mV，扫描速率 = 100 mV/s，频率 = 30 Hz，工作电极表面积 = 0.6 mm2，对流速率 = 2000 rpm。在这些优化条件下，吸附溶出伏安法（AdSV）的峰电流在5×10-7 - 6×10-6 M浓度范围内呈正比（r = 0.999）。醋丁洛尔在人血浆和尿液中的回收率分别在97 - 103%和96 - 104%范围内。该方法被证明是精确的（人血浆中日内精密度以%RSD表示，范围为2.9 - 3.2%，日间精密度以%RSD表示，范围为3.4 - 3.8%）且准确的（人尿液中日内准确度以%误差表示，范围为 -3.3 - 2.8%，日间准确度范围为 -3.3 - 1.7%）。醋丁洛尔的定量限（LOQ）和检测限（LOD）分别为1.7×10-7和5×10-7 M。研究了药物制剂中通常存在的物质可能产生的干扰，平均回收率为101.6 ± 0.64%。所开发的方波吸附溶出伏安法（SW-AdSV）的结果与参考分析方法获得的结果相当。
