甲磺酸培氟沙星的示波极谱滴定法研究

对甲磺酸培氟沙星含量的示波极谱滴定法测定进行了研究。在 pH5 2的HCl NaAc缓冲溶液中 ,四苯硼钠 (Na TPB)与甲磺酸培氟沙星作用可生成 1∶1定量沉淀 ,过滤弃去初滤液 ,用硫酸亚铊标准溶液滴定续滤液中过量的Na TPB ,通过示波极谱图 (dE/dt=f(E)曲线 )上TPB的切口消失指示滴定终点。本法操作简单、快速 ,终点直观 ,应用于多批原料药样品的测定 ,获得了满意的结果 ,其回收率为 99 4 6 %～ 1 0 0 4 % ,相对误差 <± 0 .6 % ,与部颁标准非水滴定法测得的结果基本一致。

Study on oscillopolarographic titration of pefioxacin mesylate

The determination of pefloxacin mesylate by oscillopolarographic titration was described in this paper. Pefloxacin mesylate was precipitated as PEFM-TPB in HC1-NaAc buffer solution (pH＝5.2). After filtering off the precipitate, the excessive sodium tetraphenylboron in the filtrate was titrated with thallous sulfate standard solution in an alkaline solution. The disappearance of the incision of TPB on dE/dt ＝ f (E) curve was used to indicate the end point of titration. The method was simple and rapid. The recovery rate was between 99.46% and 100.4%, the relative error was less than ± 0.60%. Experiments showed that the method had the same results as the official nonaqueous titration.