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介绍采用季铵盐 十六烷基三甲基溴化铵作滴定剂的示波极谱滴定法测定培氟沙星和环丙沙星含量的方法。在pH 4 .8HAc NaAc缓冲溶液中 ,培氟沙星和环丙沙星均能与四苯硼钠 (Na TPB)作用生成沉淀 ,干过滤后 ,用十六烷基三甲基溴化铵标准溶液代替在示波极谱滴定法中常用的有毒硫酸亚铊作为滴定剂 ,回滴滤液中过量的Na TPB ,由示波极谱图 [dE dt=f(E)曲线 ]上TPB的切口消失指示终点。本法终点直观、灵敏 ,操作简便、快速 ,应用于多批原料药样品的测定 ,均获得满意的结果 ,其回收率在 99.9%～ 10 0 .3%之间 ,最大相对误差 <± 0 .3% ,与非水滴定法测得结果基本吻合。
A method for the determination of pefloxacin and ciprofloxacin by oscillopolarographic titration using quaternary ammonium cetyltrimethylammonium bromide as titrant is introduced. Pefloxacin and ciprofloxacin were able to precipitate with sodium tetraphenylborate (Na TPB) in pH4.8HAc NaAc buffer solution. After filtration, the sample was filtered through cetyltrimethylammonium bromide Instead of using the toxic thallium sulfate commonly used in oscillopolarography as a titrant, the solution is returned to excess NaTPB in the filtrate, disappearing from the incision of the TPB on the oscillopolarography [dE dt = f (E) curve] Indicate the end point. The end of the method is intuitive, sensitive, easy to operate, fast, and is applied to the determination of multiple batches of raw drug samples, and the satisfactory results are obtained. The recovery rate is between 99.9% and 100.3%, and the maximum relative error is less than ± 0. 3%, and non-aqueous titration measured results are basically consistent.