Institute of Analytical Chemistry, Leipzig University, Linnéstraße 3, 04103 Leipzig, Germany.
Lab Chip. 2016 Nov 29;16(24):4648-4652. doi: 10.1039/c6lc01138a.
Chip-integrated, two-dimensional high performance liquid chromatography is introduced to monitor enantioselective continuous micro-flow synthesis. The herein described development of the first two-dimensional HPLC-chip was realized by the integration of two different columns packed with reversed-phase and chiral stationary phase material on a microfluidic glass chip, coupled to mass spectrometry. Directed steering of the micro-flows at the joining transfer cross enabled a heart-cut operation mode to transfer the chiral compound of interest from the first to the second chromatographic dimension. This allows for an interference-free determination of the enantiomeric excess by seamless hyphenation to electrospray mass spectrometry. The application for rapid reaction optimization at micro-flow conditions is exemplarily shown for the asymmetric organocatalytic continuous micro-flow synthesis of warfarin.
芯片集成二维高效液相色谱用于监测对映选择性连续微流合成。本文介绍了在微流控玻璃芯片上通过集成填充有反相和手性固定相材料的两种不同柱，实现二维 HPLC 芯片的首次开发，并与质谱联用。在连接转移交叉处微流的定向转向使得能够进行心切操作模式，将手性感兴趣的化合物从第一色谱维度转移到第二色谱维度。这允许通过与电喷雾质谱的无缝连接，对非对映体过量进行无干扰的测定。通过不对称有机催化连续微流合成华法林的快速反应优化实例，展示了微流条件下的应用。
