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A Microcoil NMR Probe for Coupling Microscale HPLC with On-Line NMR Spectroscopy
 

Summary: A Microcoil NMR Probe for Coupling Microscale
HPLC with On-Line NMR Spectroscopy
Raju Subramanian, Wayne P. Kelley,, Philip D. Floyd,, Zhixin J. Tan,, Andrew G. Webb,, and
Jonathan V. Sweedler*,,
Department of Chemistry, Department of Electrical and Computer Engineering, and The Beckman Institute for Advanced
Science and Technology, University of Illinois at UrbanasChampaign, 405 North Mathews Avenue, Urbana, Illinois 61801
An HPLC NMR system is presented that integrates a
commercial microbore HPLC system using a 0.5-mm
column with a 500-MHz proton NMR spectrometer using
a custom NMR probe with an observe volume of 1.1 L
and a coil fill factor of 68%. Careful attention to capillary
connections and NMR flow cell design allows on-line NMR
detection with no significant loss in separation efficiency
when compared with a UV chromatogram. HPLC NMR is
performed on mixtures of amino acids and small peptides
with analyte injection amounts as small as 750 ng; the
separations are accomplished in less than 10 min and
individual NMR spectra are acquired with 12 s time
resolution. Stopped-flow NMR is achieved by diversion
of the chromatographic flow after observation of the

  

Source: Andrews, Anne M. - Huck Institutes of the Life Sciences, Pennsylvania State University

 

Collections: Biology and Medicine