手性流动相添加法拆分酮康唑外消旋体  

Separation of ketoconazole enantiomers using high performance liquid chromatography with chiral mobile phase additives

作　　者：刘爱[1] 葛文娜[1] 吴淑燕[1] 许茜[1] 王敏[1] 殷雪琰[1] 

机构地区：[1]东南大学,江苏南京210009

出　　处：《色谱》2009年第2期240-243,共4页Chinese Journal of Chromatography

摘　　要：采用C18反相色谱柱,利用在流动相中加入手性选择剂的方法实现酮康唑对映体的拆分。研究了手性选择剂的种类及浓度、流动相pH值、甲醇比例和柱温等因素对酮康唑手性分离的影响,结果表明磺丁基-β-环糊精可以使酮康唑对映体完全分离,最后选择的流动相组成为甲醇-0.02mol/L磷酸二氢钠(体积比为60∶40,含0.02%三乙胺和1.0mmol/L磺丁基-β-环糊精,用稀磷酸调节pH值到3.00)。酮康唑对映体在6min内得到基线分离,分离度为2.05。方法简便,分离效果好,对酮康唑对映体的拆分具有应用价值。A simple and effective method for the separation of ketoconazole enantiomers was developed using the chiral mobile phase additive on a C18 reversed-phase column.Several β-cyclodextrins were investigated as chiral mobile phase additives separately.The results showed that ketoconazole enantiomers were well separated by only adding sulfobutyl ether-β-cyclodextrin（SBE-β-CD） into the mobile phase.Excellent enantioseparation was achieved with the mobile phase composed of methanol-0.02 mol/L NaH2PO4（60∶40,v/v,containing 1.0 mmol/L SBE-β-CD and 0.02% triethylamine,at pH 3.00 adjusted with phosphoric acid aqueous solution）.The flow rate was 1.0 mL/min.The detection wavelength was set at 225 nm and the column temperature at 30 ℃.Under the optimized conditions,the resolution of ketoconazole enantiomers was 2.05.

关 键 词：高效液相色谱法 酮康唑对映体 磺丁基-β-环糊精 手性流动相添加剂 

分 类 号：O658[理学—分析化学]