流动注射-分光光度法测定药物中克林霉素磷酸酯的含量
FI-Spectrophotometric Determination of Clindamycin Phosphate in Drugs
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摘要: 试验表明:在pH 3.8的乙酸盐缓冲介质中,克林霉素磷酸酯(CLP)能将铁(Ⅲ)还原为铁(Ⅱ),而所生成的铁(Ⅱ)与邻菲啰啉反应生成有色络合物(λmax=508 nm),且生成的铁(Ⅱ)量与CLP之间存在定量关系,经换算所测得吸光度与CLP的质量浓度在0.70~140 mg·L-1之间呈线性关系。据此并结合流动注射技术(FI)提出了FI-分光光度法间接测定药物中CLP的新方法优化的分析条件如下:① 乙酸盐缓冲溶液的加入量:2.5 mL;② 铁(Ⅲ)溶液质量浓度:10.0 mg·L-1;③ 邻菲啰啉溶液浓度:1.5×10-3mol·L-1;④ 反应温度:85 ℃。该方法的检出限为0.060 mg·L-1。应用此方法测定了药物中CLP的含量,测定值与国家药品标准方法的测定值相符。Abstract: It was found that in an acetate buffer medium of pH 3.8, Fe(Ⅲ) ion was reduced to Fe(Ⅱ) ion by clindamycin phosphate (CLP) which in turn reacted with o-phenanthroline solution to form a colored complex (λmax=508 nm) and that linear relationship was kept between values of absorbance and mass concentration of CLP [calculated indirectly from the amount of Fe(Ⅱ) ion found] in the range of 0.70-140 mg·L-1. Based on this fact and by applying the FIA technique, an indirect FI-spectrophotometric method for determination of CLP was proposed. The optimum analytical conditions found were as follows: ① amount of the acetate buffer solution added: 2.5 mL; ② mass concentration of Fe(Ⅲ) solution: 10.0 mg·L-1; ③ concentration of o-phenanthroline solution: 1.5×10-3mol·L-1; ④ temperature of reaction: 85 ℃. Detection limit (3s/k) of the method found was 0.060 mg·L-1. The proposed method was applied to determination of CLP in drug samples, giving results in consistency with those found by the method of national standard of drugs.