Enantioselective reaction monitoring utilizing two-dimensional heart-cut liquid chromatography on an integrated microfluidic chip.
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.
Institute of Analytical Chemistry, Leipzig University, Linnéstraße 3, 04103 Leipzig, Germany. belder@uni-leipzig.de.
Carsten
C
Lotter
Institute of Analytical Chemistry, Leipzig University, Linnéstraße 3, 04103 Leipzig, Germany. belder@uni-leipzig.de.
Elisabeth
E
Poehler
Institute of Analytical Chemistry, Leipzig University, Linnéstraße 3, 04103 Leipzig, Germany. belder@uni-leipzig.de.
Josef J
JJ
Heiland
Institute of Analytical Chemistry, Leipzig University, Linnéstraße 3, 04103 Leipzig, Germany. belder@uni-leipzig.de.
Laura
L
Mauritz
Institute of Analytical Chemistry, Leipzig University, Linnéstraße 3, 04103 Leipzig, Germany. belder@uni-leipzig.de.
Detlev
0000-0001-6295-8706
D
Belder