在环糊精修饰的整体柱上通过毛细管电色谱法进行对映体分离。
Enantiomer separation by capillary electrochromatography on a cyclodextrin-modified monolith.
作者信息
Wistuba D, Schurig V
机构信息
Institute of Organic Chemistry, University of Tübingen, Germany.
出版信息
Electrophoresis. 2000 Sep;21(15):3152-9. doi: 10.1002/1522-2683(20000901)21:15<3152::AID-ELPS3152>3.0.CO;2-L.
A chiral monolithic stationary phase was prepared by packing a capillary with bare porous silica and sintering the silica bed at high temperature. The resulting silica monolith was polymer-coated with Chirasil-Dex, a permethylated beta-cyclodextrin covalently linked via an octamethylene spacer to dimethylpolysiloxane. Subsequently, Chirasil-Dex was thermally immobilized on the silica support and a chiral monolith of very high stability (30 kV, more than 400 bar pressure) was obtained. The enantiomer separation of various chiral compounds by monolithic (rod) capillary electrochromatography (rod-CEC) was feasible. This method was compared with capillary liquid chromatography (LC) in a single-column mode using unified equipment. About two to three times higher efficiency was found in the rod-CEC mode as compared to rod-LC. The influence of pressure-driven flow support on efficiency, resolution, elution time and baseline stability was investigated. The amount and nature of organic modifier strongly influences efficiency and resolution.
通过将毛细管填充裸露的多孔二氧化硅并在高温下烧结二氧化硅床来制备手性整体固定相。所得的二氧化硅整体用Chirasil-Dex进行聚合物涂覆，Chirasil-Dex是一种通过八亚甲基间隔基与二甲基聚硅氧烷共价连接的全甲基化β-环糊精。随后，将Chirasil-Dex热固定在二氧化硅载体上，得到了稳定性非常高（30 kV，超过400 bar压力）的手性整体。通过整体（棒状）毛细管电色谱（棒状CEC）对各种手性化合物进行对映体分离是可行的。使用统一设备以单柱模式将该方法与毛细管液相色谱（LC）进行了比较。与棒状LC相比，在棒状CEC模式下发现效率高出约两到三倍。研究了压力驱动流支持对效率、分辨率、洗脱时间和基线稳定性的影响。有机改性剂的量和性质强烈影响效率和分辨率。
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