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.
出处
《色谱》
CAS
CSCD
北大核心
2014年第8期880-885,共6页
Chinese Journal of Chromatography
基金
国家自然科学基金项目(21276080)
关键词
高效液相色谱
手性固定相
手性拆分
氨鲁米特
high performance liquid chromatography （HPLC）
chiral stationary phase
chiralresolution
aminoglutethimide
