文献类型：期刊文献

中文题名：纤维素-三(3,5-二甲苯基氨基甲酸酯)手性固定相拆分氨鲁米特对映体

英文题名：Chromatographic separation of aminoglutethimide enantiomers on cellulose tris(3,5-dimethylphenylcarbamate)chiral stationary phase

作者：林小建[1];龚如金[1];李平[1];于建国[1]

机构：[1]华东理工大学化工学院,化学工程联合国家重点实验室,上海200237

年份：2014

卷号：32

期号：8

起止页码：880

中文期刊名：色谱

外文期刊名：Chinese Journal of Chromatography

收录：CSTPCD;;Scopus;WOS:【ESCI(收录号:WOS:000434538200015)】；北大核心:【北大核心2011】；CSCD:【CSCD2013_2014】；PubMed;

基金：国家自然科学基金项目(21276080)

语种：中文

中文关键词：高效液相色谱;手性固定相;手性拆分;氨鲁米特

外文关键词：high performance liquid chromatography(HPLC);chiral stationary phase;chiralresolution;aminoglutethimide

摘要：以纤维素-三(3,5-二甲苯基氨基甲酸酯)为手性固定相(Chiralcel OD-H)在高效液相色谱上拆分了氨鲁米特对映体。通过测定氨鲁米特在正己烷/乙醇和正己烷/异丙醇中的溶解度,优选了对样品溶解度大的流动相体系,并考察了流动相添加剂乙醇胺对拆分效果的影响。在此基础上进一步研究了流动相中乙醇含量、柱温和进样量对分离因子、分离度、不对称因子和理论板数的影响,从而确定了最佳的拆分条件:固定相为Chiralcel OD-H,流动相为正己烷/乙醇/乙醇胺(体积比为30∶70∶0.1),柱温25℃。本文所得结果可为工业放大提供基础数据。
Aminoglutethimide(AG)has been used clinically as a drug in the treatment of hor-mone-dependent metastatic breast cancer.It was reported that S-(-)-AG enantiomer had small activity and sometimes might cause side effects.Therefore,it was of great significance to obtain the high-purity R-(+)-AG by enantioseparation.In this work,aminoglutethimide enanti-omers were separated by high performance liquid chromatography(HPLC)using an analytical column which was packed with cellulose tris(3,5-dimethylphenylcarbamate)stationary phase(ChiralcellOD-H).The solubilities of racemic AG in two different solvent compositions,n-hex-ane/ethanol and n-hexane/isopropanol,were measured,separately.The effects of alcohol con-tent and monoethanolamine additive on the separation performance of racemic AG by HPLC were investigated.According to the experiments,n-hexane-ethanol(30:70,v/v)with 0.1%monoethanolamine additive was selected as the mobile phase.The separation factor,resolu-tion,asymmetry factor,number of theoretical plates and maximum column capacity were measured and analyzed for the chromatographic separation of racemic AG at a flow-rate of 0.6 mL/min and column temperature of 25-40℃,with ChiralcellOD-H as stationary phase and n-hexane-ethanol(30:70,v/v)with 0.1%monoethanolamine as mobile phase.This work pro-vides the basic information of chromatographic separation for the batch and continuous produc-tion of aminoglutethimide enantiomers.