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.
出处
《色谱》
CAS
CSCD
北大核心
2009年第2期240-243,共4页
Chinese Journal of Chromatography
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
high performance liquid chromatography(HPLC)
ketoconazole enantiomers
sulfobutyl ether-β-cyclodextrin
chiral mobile phase additives