CE-ECL法同时测定复方磷酸可待因中三种成分的方法学研究

Methodology research on determination of three ingredients in compound codeine phosphate solution by CE-ECL

目的建立毛细管电泳-电化学发光法分离并检测复方磷酸可待因中三种成分,磷酸可待因、马来酸溴苯那敏和盐酸麻黄碱含量的新方法。方法基于碱性介质中,复方磷酸可待因溶液中三种主要成分对联吡啶钌在铂电极上的电化学发光信号的增敏作用,且增敏强度和药物浓度成线性关系,与毛细管电泳联用,建立了毛细管电泳-电化学发光法分离并检测其含量的新方法。结果在优化的实验条件下,确定三种药物对照品的线性范围、线性方程和检出限。通过对浓度为1.0×10-5kg/L的磷酸可待因、马来酸溴苯那敏和盐酸麻黄碱对照品进行12次平行测定,其ECL发光强度的RSD值分别为2.89%,3.76%,3.32%。结论该方法可用于复方磷酸可待因口服溶液中三种主要成分的含量测定,待测样品中的基质不干扰测定,方法的回收率分别为100.4%,101.9%,99.8%(n=5)。

Objective To establish a novel method for simultaneous determination of three ingredients （codeine phosphate, brompheniramine maleate and ephedrine hydrochloride） in compound codeine phosphate solution by using capillary electrophoresis （CE） coupled with electrochemiluminescence （ECL）. Methods Based on enhanced ECL intensity of tris （2,2＇-bypyridine） ruthenium （Ⅱ） with codeine phosphate, brompheniramine maleate and ephedrine hydrochloride, as well as the linear correlation between enhanced sensitivity intensity and drug concentration, platinum disk （300 μm in diameter） was used as a working electrode. Parameters affecting separation and detection were optimized. Results Under the optimized conditions, we determined the linear range, regression equation and detection limit for the three ingredients. The relative standard deviation of ECL intensity for twelve consecutive injections of 1.0 × 10^-5 kg/L standard sample of three kinds of drug was 2.89% for codeine phosphate, 3.76% for brompheniramine maleate and 3.32% for ephedrine hydrochloride, respectively. Satisfactory results were obtained without interference from sample matrixes. Conclusion The method was successfully applied to the determination of three ingredients in oral solution of compound codeine phosphate, with the recovery rate of 100. 4% for codeine phosphate, 101. 9% for brompheniramine maleate and 99. 8% for ephedrine hydrochloride.