摘要
1,5-萘二酚(1,5-dihydroxynaphthalene,DOP)和5-羟基萘满酮(5-hydroxy-1-tetralone,HOT)是合成丁萘酮心安(bunolol)的中间体,而HOT又是由DOP催化氢化还原得到的,反应过程受到温度、压力、催化剂等因素的影响,其中氢化反应是合成丁萘酮心安最关键的步骤。为了选择最佳反应条件。
A reversed phase high performace liquid chromatographic method was developed for the separation and simultaneous determination of 1,5-dihydroxynaphthalene (DOP) and 5-hydroxy-1-tetralone (HOT).The column (ODS 150×4mm,5μ) was eluted with 1:1 of methanol and water solution (containing 1 % acetic acid) at 0.5ml / min as mobile phase and acetophenone as internal standard.The fractions were monitored by UV-detector at 317nm.Good linearities were obtained in the rang of 0.02-0.4μg for DOP (γ=0.999) and 0.04-0.8μg,for HOT (γ=0.999).The detection limits of the two compounds were found to be 1 ng and 3 ng respectively.The average recoveries were 100.2% (DOP) and 98.38 (HOT) respectively.The results were satisfactory for the quantitative determination and the control of the catalytic hydrogenation of DOP.
出处
《色谱》
CAS
CSCD
北大核心
1991年第1期57-59,共3页
Chinese Journal of Chromatography