Zhang Yingru, Dai Jun, Wang-Iverson David B, Tymiak Adrienne A
Bioanalytical and Discovery Analytical Science, Pharmaceutical Research Institute, Bristol-Myers Squibb Company, Princeton, NJ 08648, USA.
Chirality. 2007 Sep;19(9):683-92. doi: 10.1002/chir.20409.
This article describes a very useful extension of an unique column switching technique called "Simulated Moving Columns" (SMC) that was previously reported for chiral high performance liquid chromatography (HPLC) (Zhang and McConnell, Journal of Chromatography A 2004;1028:227-238). SMC uses two or three short chiral columns connected in series, and enables the unresolved enantiomers to separate repeatedly and exclusively through each of the columns until sufficient resolution is attained. The technique is significantly enhanced through the use of supercritical fluid chromatography (SFC). The supercritical or near critical carbon dioxide (CO(2)) used in the mobile phase of SFC possesses the properties of a liquid as well as a gas, and usually results in much sharper peaks compared to HPLC. Consequently, by combining SMC with SFC (SMC-SFC), we were able to dramatically increase the number of SMC cycles with significantly less band broadening compared to HPLC. For the first time, an enantioselective SFC separation was demonstrated by increasing the column from the actual 20 cm length to reach a half meter virtual length with remarkably enhanced efficiency. Off-column band broadening resulting from a two-column SMC system was measured, and its impact on the enantioselectivity of SMC-SFC was found to be much less than in SMC-HPLC.
本文介绍了一种独特的柱切换技术——“模拟移动柱”(SMC)的非常有用的扩展。该技术先前已报道用于手性高效液相色谱(HPLC)(Zhang和McConnell,《色谱杂志A》2004年;1028:227 - 238)。SMC使用两根或三根串联的短手性柱,能使未分离的对映体通过每根柱子反复且唯一地进行分离,直至获得足够的分离度。通过使用超临界流体色谱(SFC),该技术得到显著增强。SFC流动相中使用的超临界或近临界二氧化碳(CO₂)兼具液体和气体的特性,与HPLC相比,通常能产生尖锐得多的峰。因此,通过将SMC与SFC相结合(SMC - SFC),与HPLC相比,我们能够显著增加SMC循环次数,且峰展宽明显更小。首次通过将实际长度为20 cm的柱子增加到半米的虚拟长度,以显著提高效率,实现了对映体选择性SFC分离。测量了两柱SMC系统导致的柱外峰展宽,发现其对SMC - SFC对映选择性的影响远小于SMC - HPLC。