Ghoneim M M, Abushoffa A M, Moharram Y I, El-Desoky H S
Chemistry Department, Faculty of Science, Tanta University, 31527 Tanta, Egypt.
J Pharm Biomed Anal. 2007 Jan 17;43(2):499-505. doi: 10.1016/j.jpba.2006.07.049. Epub 2006 Sep 6.
The electrochemical behavior of norethisterone at the mercury electrode was studied in the universal buffer of various pH values using dc-polarography, cyclic voltammetry and controlled-potential electrolysis. Norethisterone was reduced at the mercury electrode via the consumption of two electrons corresponding to reduction of the 3-keto-delta-4-group in the A-ring of the molecule. The pK(a) value (8.7) of norethisterone was determined from the polarographic and spectrophotometric measurements. A fully validated, simple, sensitive, precise and inexpensive square-wave adsorptive cathodic stripping (SWAdCS) voltammetry procedure was described for trace quantification of bulk norethisterone. The stripping voltammetry peak current of norethisterone in a universal buffer of pH 5 following its accumulation onto the hanging mercury drop electrode (HMDE) at -0.6 V (versus Ag/AgCl/KCl(s)) for 130 s showed a linear response with the concentration over the range 5 x 10(-9) to 3 x 10(-7)M norethisterone. Detection and quantitation limits of 1.5 x 10(-9) and 5 x 10(-9)M bulk norethisterone, respectively, were achieved. The proposed procedure was successfully applied for the assay of norethisterone in Steronate tablets without interference from excipients.
使用直流极谱法、循环伏安法和控制电位电解法,在不同pH值的通用缓冲液中研究了炔诺酮在汞电极上的电化学行为。炔诺酮在汞电极上通过消耗两个电子而被还原,这与分子A环中3-酮-δ-4-基团的还原相对应。通过极谱法和分光光度法测量确定了炔诺酮的pK(a)值(8.7)。描述了一种经过充分验证的、简单、灵敏、精确且廉价的方波吸附阴极溶出伏安法(SWAdCS),用于痕量定量分析大量炔诺酮。炔诺酮在pH 5的通用缓冲液中,于-0.6 V(相对于Ag/AgCl/KCl(s))在悬汞滴电极(HMDE)上富集130 s后,其溶出伏安法峰电流与炔诺酮浓度在5×10(-9)至3×10(-7)M范围内呈线性响应。分别实现了大量炔诺酮的检测限和定量限为1.5×10(-9)和5×10(-9)M。所提出的方法成功应用于测定炔诺酮片,不受辅料干扰。