Hydrogen/deuterium exchange using a coaxial sheath-flow interface for capillary electrophoresis/mass spectrometry

The interfacing of capillary electrophoresis (CE) with mass spectrometry (MS) is well established and may be accomplished by use of either a coaxial arrangement or by employing a liquid T‐junction. In both these interfaces a make‐up flow is introduced. This is required because of the mismatch in flow rates for capillary electrophoresis ∼nL/min and ‘true’ electrospray ∼2–10 µL/min. Electrical connectivity may also be established where the liquid flows meet (the introduction of nanospray renders the use of make‐up flow unnecessary). Hydrogen/deuterium (H/D) exchange occurs in solution when there are labile hydrogen atoms present in a molecule. The establishment of the presence and the number of such exchangeable hydrogen atoms may be of importance in the identification and differentiation of compounds. It may also be an aid in the structural elucidation of unknown materials. We have investigated the feasibility of carrying out H/D exchange via a CE/MS interface. This involved the addition of D2O to the sheath flow and our preliminary results showing the separations of drug substances, subsequently undergoing exchange, are presented. Copyright © 2000 John Wiley & Sons, Ltd.