Bezhitashvili Lia, Bardavelidze Anna, Ordjonikidze Teona, Chankvetadze Lali, Chity Mike, Farkas Tivadar, Chankvetadze Bezhan
Institute of Physical and Analytical Chemistry, School of Exact and Natural Sciences, Tbilisi State University, Chavchavadze Ave 3, 0179 Tbilisi, Georgia.
Phenomenex Inc., 411 Madrid Ave., Torrance, 90501 CA, USA.
J Chromatogr A. 2017 Jan 27;1482:32-38. doi: 10.1016/j.chroma.2016.12.055. Epub 2016 Dec 29.
Our earlier studies on the preparation of chiral stationary phases (CSP) based on superficially porous (or core-shell) silica (SPS) particles for the separation of enantiomers in HPLC have provided proof to the advantages of such sorbents. In particular, higher enantioselectivity was observed with the columns packed with superficially porous CSP compared to the columns packed with fully-porous (FP) silica-based CSPs at comparable content of chiral selector (polysaccharide derivative) in CSP. Also, less dependence of plate height on mobile phase flow rate and higher plate numbers and resolution calculated per unit time (i.e. speed of separation) were observed with SPS-based CSPs. Thirty years of CSP development have demonstrated that wide-pore silica has to be used as a support for large molecular weight chiral selectors such as the ones based on polysaccharides. In this study the effect of pore size of the core-shell silica support and of other experimental factors on column performance is demonstrated. Reduced plate heights in the range 1.4-1.5 were obtained, as well as highly effective baseline separations of enantiomers were observed with analysis times of less than 15s.
我们早期关于制备基于表面多孔（或核壳）硅胶（SPS）颗粒的手性固定相（CSP）用于高效液相色谱法拆分对映体的研究，已证实了此类吸附剂的优势。特别是，在手性固定相中手性选择剂（多糖衍生物）含量相当的情况下，与填充全多孔（FP）硅胶基手性固定相的色谱柱相比，填充表面多孔手性固定相的色谱柱表现出更高的对映体选择性。此外，基于表面多孔硅胶的手性固定相还表现出板高对流动相流速的依赖性较小，以及每单位时间计算得到的板数和分离度更高（即分离速度更快）。三十年来手性固定相的发展表明，必须使用大孔硅胶作为基于多糖等大分子手性选择剂的载体。在本研究中，展示了核壳硅胶载体的孔径以及其他实验因素对色谱柱性能的影响。获得了1.4 - 1.5范围内的折合板高，并且观察到对映体在不到15秒的分析时间内实现了高效基线分离。
