敌草胺对映体的高效液相色谱分离及手性拆分热力学研究

周瑛; 张世浩; 刘维屏; 陈易晖; 叶丽

敌草胺对映体的高效液相色谱分离及手性拆分热力学研究

Enantioresolution and Study of Thermodynamical Property of Napropamide by High Performance Liquid Chromatography

摘要

摘要: 利用直链淀粉三-(3,5-二甲基苯基氨基甲酸酯)手性固定相(AD-RH柱)和纤维素三-(3,5-二甲基苯基氨基甲酸酯)手性固定相(OD-RH柱),以乙腈-水为流动相,对敌草胺对映体进行了直接手性拆分研究。考察了流动相组成、流速、柱温等对敌草胺对映体的色谱保留和分离的影响,并对敌草胺对映体与固定相之间的色谱保留和分离的热力学机理进行了讨论。结果表明,在流速为0.5mL/m in、乙腈-水为50∶50(体积比)、柱温在1035℃条件下,AD-RH和OD-RH柱的△△H0值分别为-1 160.79和-673.40J/mol,即AD-RH柱的拆分能力优于OD-RH柱,二者都能实现基线分离。

Abstract: The enantiomer of napropamide was resolved under reverse phase high performance liquid chromatography(HPLC) using Chiralcel(AD-RH) and Chiralcel OD-RH with acetonitrile-water as a mobile phase.The effects of the content of acetonitrile in mobile phase,flow-rate and temperature on the chiral separation of napropamide were studied.The chiral separation mechanism of napropamide enantiomer on the CSPs was analysed by thermodynamical parameters.The results showed that the △△H0 of ADRH and OD-RH chiral column were-1 160.79 J/mol and-673.40 J/mol respectively,namely the stereoselectivity of Chiralcel AD-RH was better than Chiralcel OD-RH and good enantiomeric separations were achieved with both CSPs under the experiment of flow-rate 0.5 mL/min,acetonitrile-water 50 ∶50 in volume and temperature 10～35℃.

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