异丙甲草胺立体异构体在高效液相色谱手性固定相上的分离

Stereoisomeric Separation of Metolachlor by High Performance Liquid Chromatography Chiral Stationary Phase

在Pirkle“刷型”(S ,S) Whelk O1手性柱和涂敷型纤维素三 (3,5 二甲基苯基氨基甲酸酯 ) (CDMPC)手性柱上 ,对异丙甲草胺立体异构体进行了分离。在 (S ,S) Whelk O1手性柱上考察了不同体积比的正己烷 异丙醇流动相对分离的影响 ,发现当异丙醇含量降低时有利于异构体的分离 ;在CDMPC手性柱上考察了正己烷中醇类改性剂的种类和浓度对分离的影响 ,发现醇含量降低时和采用大体积的醇时有利于异构体的分离。异丙甲草胺的对映异构体之间在 (S ,S) Whelk O1手性柱上获得了分离 ,在CDMPC手性柱上分离出了异丙甲草胺 4个异构体中的 3个。同时测定了富S 异丙甲草胺异构体中S 异构体的过量值 (EE) ,本方法可用于富S

The stereoisomers of metolachlor were separated on self-prepared cellulose tris-(3,5-dimethylphenylcarbamate)(CDMPC) chiral column and Pirkle brush-type (S,S)-Whelk-O1 chiral column. The separation were made under normal phase with a mobile phase of n-hexane-alcohol (ethanol,2-propanol, n-butanol, s-butanol, tert-butanol) in various proportions. The mobile phase was optimized to achieve the best resolution. On CDMPC got three out of four stereoisomers separation, and got two enantiomeric pairs of diastereomers. Effects of variation of alcohol concentration were studied, meantime the excess of the 1′S-isomers over the 1′R-isomers was calculated, and the results show that this method is suitable for the quantity of rich 1′S-metolachlor.