Institute of Physical and Analytical Chemistry, School of Exact and Natural Sciences, Tbilisi State University, Chavchavadze Ave 3, 0179 Tbilisi, Georgia.
J Chromatogr A. 2012 Apr 20;1234:50-5. doi: 10.1016/j.chroma.2012.01.084. Epub 2012 Feb 3.
This article reports comparative high-performance liquid chromatographic separations of enantiomers with chiral stationary phases (CSPs) prepared by coating cellulose tris(4-chloro-3-methylphenylcarbamate) on totally porous and on core-shell type silica of comparable particle diameter. Several interesting observations were made: (1) the selectivity of separation was higher on core-shell type CSP compared to totally porous CSP at comparable content of chiral selector (polysaccharide derivative); (2) much flatter dependence of plate height on the mobile phase flow rate was observed for columns packet with CSP prepared with core-shell silica compared to the ones packed with CSPs prepared with totally porous particles; (3) at low mobile phase flow rates core-shell CSP provided lower resolving ability compared to a commercially available CSP having four times higher content of chiral selector along with higher retention of chiral analytes. However, at high flow rates core-shell type CSP performed similarly or better than the commercial column in regards of plate count (N) and peak resolution (R(s)) per column length and within a given total analysis time. The advantage of CSP prepared with core-shell silica is obvious from the viewpoint of plate numbers and resolution calculated per unit time (i.e. speed of analysis).
本文报道了用纤维素三(4-氯-3-甲基苯基碳酸酯)涂敷在全多孔和核壳型硅胶(粒径相当)上制备的手性固定相(CSP)对映体的高效液相色谱拆分比较。观察到了几个有趣的现象:(1)在可比手性选择剂(多糖衍生物)含量下,核壳型 CSP 的分离选择性高于全多孔型 CSP;(2)与用全多孔颗粒填充的 CSP 相比,用核壳型硅胶制备的 CSP 填充的色谱柱的板高对流动相流速的依赖性更平坦;(3)在低流动相流速下,核壳型 CSP 的分辨率低于市售的具有四倍更高手性选择剂含量和更高手性分析物保留的 CSP。然而,在高流速下,核壳型 CSP 在柱长和给定的总分析时间内的板数(N)和峰分辨率(R(s))方面与商业柱的性能相当或更好。从单位时间内的板数和分辨率(即分析速度)的角度来看,用核壳型硅胶制备的 CSP 的优势是显而易见的。