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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

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【作者】 刘爱葛文娜吴淑燕许茜王敏殷雪琰

【Author】 LIU Ai,GE Wenna,WU Shuyan,XU Qian,WANG Min,YIN Xueyan(Southeast University,Nanjing 210009,China)

【机构】 东南大学

【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。

【Abstract】 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.

  • 【文献出处】 色谱 ,Chinese Journal of Chromatography , 编辑部邮箱 ,2009年02期
  • 【分类号】R917
  • 【被引频次】19
  • 【下载频次】363
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