Lau O W, Cheung Y M
Department of Chemistry, Chinese University of Hong Kong, Shatin, N.T.
Analyst. 1990 Oct;115(10):1349-53. doi: 10.1039/an9901501349.
A simple, efficient and accurate gas-liquid chromatography (GLC) method for the simultaneous determination of eight active ingredients in cough-cold syrups has been developed. The active ingredients under study were bromhexine, chlorpheniramine, codeine, dextromethorphan, diphenhydramine, ephedrine/pseudoephedrine, guaiphenesin and papaverine. Before injection, the active ingredients were first separated, from the excipients present in the cough-cold syrups, with chloroform, from alkaline medium. They were then separated by GLC on a glass column (5 ft x 2 mm i.d.) packed with 3% of OV-25 supported on Supelcoport (80-100 mesh). The column temperature was maintained at 170 degrees C for 1 min, then programmed to 265 degrees C at a rate of 10 degrees C min-1, and maintained at this temperature for 10 and 1 min, respectively, for samples with and without papaverine. The flow-rate of the nitrogen carrier gas was 30 ml min-1. A flame-ionisation detector was used for detection, and clomipramine hydrochloride was used as the internal standard. The recoveries of the drugs ranged from 96.0 to 99.7%, and the relative standard deviations for ten replicate determinations ranged from 0.49 to 4.7%. Results are reported for nine commercially available cough-cold syrups.
已开发出一种简单、高效且准确的气相色谱法（GLC），用于同时测定止咳感冒糖浆中的八种活性成分。所研究的活性成分有溴己新、氯苯那敏、可待因、右美沙芬、苯海拉明、麻黄碱/伪麻黄碱、愈创甘油醚和罂粟碱。进样前，先在碱性介质中用氯仿将活性成分与止咳感冒糖浆中的辅料分离。然后在填充有3%涂覆于Supelcoport（80 - 100目）上的OV - 25的玻璃柱（5英尺×2毫米内径）上通过GLC进行分离。柱温在170℃保持1分钟，然后以10℃/分钟的速率程序升温至265℃，对于含和不含罂粟碱的样品，分别在此温度下保持10分钟和1分钟。氮气载气的流速为30毫升/分钟。使用火焰离子化检测器进行检测，并以盐酸氯米帕明作为内标。药物的回收率在96.0%至99.7%之间，十次重复测定的相对标准偏差在0.49%至4.7%之间。报告了九种市售止咳感冒糖浆的结果。
