Dual microcoil NMR probe coupled to cyclic CE for continuous separation and analyte isolation

Dimuthu A. Jayawickrama, Jonathan V. Sweedler

Research output: Contribution to journalArticlepeer-review

Abstract

Capillary electrophoresis (CE)-nuclear magnetic resonance (NMR) spectroscopy combines the separation efficiency of CE and the information-rich detection capabilities of NMR. However, the temporally narrow CE peaks reduce NMR sensitivity and prevent on-line multidimensional NMR acquisitions. In this work, cyclic CE with multicoil NMR instrumentation is developed to perform CE in multiple closed loops. As a proof of concept, a two-loop five-junction capillary configuration creates two connected yet independently operable fluidic loops. With appropriate voltage switching, analytes can be directed as desired around or between the loops, and a particular analyte band can be parked in one NMR detector coil while CE continues in the second loop and monitored with a second NMR detector coil. The separation of a mixture of amino acids (Ala, Val, Thr) is achieved in two cycles. After one CE cycle, Ala is separated and COSY data are recorded in one loop while Val and Thr are separated in the second loop. At the end of the second cycle, both Val and Thr are separated and multidimensional NMR spectra acquired. With this instrumentation and appropriate protocols, two-dimensional NMR data acquisition and CE separation are achieved simultaneously.

Original languageEnglish (US)
Pages (from-to)4894-4900
Number of pages7
JournalAnalytical Chemistry
Volume76
Issue number16
DOIs
StatePublished - Aug 15 2004

ASJC Scopus subject areas

  • Analytical Chemistry

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