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Enantiomeric separation of the key intermediate of nebivolol using supercritical fluid chromatography
Author(s): 
Pages: 642-645
Year: Issue:  11
Journal: Qilu Pharmaceutical Affairs

Keyword:  超临界流体色谱法奈必洛尔手性中间体手性分离6-氟-34-二氢2H-1-苯并吡喃-2-甲酸;
Abstract: 目的 建立奈必洛尔关键手性中间体6-氟-3,4-二氢2H-1-苯并吡喃-2-甲酸的超临界流体色谱法(SFC).方法 采用分析型超临界流体色谱法结合大赛璐Chiralpak IG(4.6 mm×150 mm,5μm)手性色谱柱直接拆分该手性中间体,分别考察了固定相的种类、改性剂的种类及比例、流速、温度和背压等因素对手性分离的影响.结果 建立了分析型的色谱拆分条件:流动相为超临界CO2-甲醇(75:25,V/V),流速为2.0 mL?min-1,检测波长为220 nm;柱温为308 K,背压为100 bar.结论 该方法对映体分离度好(4.22),保留时间短,适合分析及制备放大.
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