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

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。

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

Aminoglutethimide (AG) has been used clinically as a drug in the treatment of hormone-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 enantiomers were separated by high performance liquid chromatography (HPLC) using an analytical column which was packed with cellulose tris(3,5-dimethylphenylcarbamate) stationary phase (Chiralcel OD-H). The solubilities of racemic AG in two different solvent compositions, n-hexane/ethanol and n-hexane/isopropanol, were measured, separately. The effects of alcohol content 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, resolution, 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 Chiralcel OD-H as stationary phase and n-hexane-ethanol (30:70, v/v) with 0.1% monoethanolamine as mobile phase. This work provides the basic information of chromatographic separation for the batch and continuous production of aminoglutethimide enantiomers.