摘要
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。
This paper describes the determination of pefloxacin and ciprofloxacin by oscillopolarographic titration with cetyltrimethylammonium bromide (CTMAB) as titrant. Sodium tetraphenylborate (Na TPB) is added to precipitate pefloxacin and ciprofloxacin in HAc NaAc buffer solution (pH=4.8). After filtering, the excess of TPB in the filtrate was titrated by substituting CTMAB standard solution, which was used instead of poisonous thallous sulfate as titrant. The disappearance of the incision of TPB on d E /d t=f(E ) curve was used to indicate the end point of the titration. The method is simple and rapid. It has been applied to the determination of pefloxacin and ciprofloxacin raw materials with satisfactory results. The recovery was from 99.9% to 100.3% and the relative error was less than ±0.3%. Experiments showed that the method gave the same results as the approach using nonaqueous titration.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2002年第4期454-457,共4页
Chinese Journal of Analytical Chemistry
