Institute of Chemical Methodologies, Consiglio Nazionale delle Ricerche, Area della Ricerca di Roma I, Via Salaria Km 29,300, 00015 Monterotondo, Roma, Italy.
Institute of Chemical Methodologies, Consiglio Nazionale delle Ricerche, Area della Ricerca di Roma I, Via Salaria Km 29,300, 00015 Monterotondo, Roma, Italy.
J Chromatogr A. 2014 Oct 10;1363:363-71. doi: 10.1016/j.chroma.2014.05.029. Epub 2014 May 17.
In this study the separation performance of various chiral stationary phases (CSPs) made of polysaccharide-based chiral selectors coated onto superficially porous (core-shell or fused-core) silica supports were evaluated. The CSPs obtained by coating of various amounts of chiral selector (1-5%) onto supports of various pore size (100 and 300 Å) were studied. Their evaluation was pursued in both chiral nano-liquid chromatography (nano-LC) and chiral capillary electrochromatography (CEC). Among the goals of this study was to re-examine our previous unexpected finding of better performance of superficially porous CSP under CEC conditions compared to nano-LC conditions for a new set of chiral compounds, as well as to study the effect of varying the chiral selector content and nominal pore size of supporting silica on the performance of core-shell silica-based polysaccharide-type CSPs. Based on the results of this study it can be seen that CSPs based on superficially porous silica can successfully be used for the separation of enantiomers in both nano-LC and CEC mode. Only a slight advantage of CEC over nano-LC mode was observed in this study from the viewpoint of plate numbers, especially at higher mobile phase flow rates. It must also be noted that the optimal theoretical plate height is still too high and further optimization of superficially porous CSPs is necessary for both nano-LC and CEC applications.
在这项研究中,评估了涂覆在表面多孔(核壳或融合核)硅胶载体上的基于多糖的手性选择剂的各种手性固定相(CSP)的分离性能。研究了通过将不同量的手性选择剂(1-5%)涂覆在不同孔径(100 和 300Å)的载体上来获得的 CSP。在手性纳流液相色谱(nano-LC)和手性毛细管电色谱(CEC)中均对其进行了评估。这项研究的目标之一是重新检查我们以前在新的一组手性化合物的情况下,在 CEC 条件下与 nano-LC 条件相比,表面多孔 CSP 的性能更好的意外发现,以及研究手性选择剂含量和支撑硅胶的标称孔径变化对核壳型硅胶基于多糖型 CSP 性能的影响。基于这项研究的结果,可以看出基于表面多孔硅胶的 CSP 可以成功地用于在 nano-LC 和 CEC 模式下分离对映体。从理论塔板数的角度来看,尤其是在较高的流动相流速下,本研究仅观察到手性电色谱模式相对于纳流液相色谱模式略有优势。还必须注意的是,最佳理论塔板高度仍然过高,对于 nano-LC 和 CEC 应用,均有必要对手性表面多孔 CSP 进行进一步优化。