An NMR method of analyzing an analyte comprises feeding an analyte sample
fluid to an NMR flow cell. The NMR flow cell comprises an RF microcoil
operably associated with an enlarged containment region. The mobile phase
of the analyte sample flowing through the NMR flow cell has a solvent
gradient greater than 10% per minute. The analyte sample fluid can be fed
to the NMR flow cell from an analyte extraction chamber, e.g., operative
to perform liquid chromatography, capillary electrophoresis, or the like,
especially a capillary-based analyte extraction chamber integrated in an
NMR probe with the NMR flow cell. A sample volume is held in the NMR flow
cell for equilibration less than 1 hour, preferably less than 30 minutes
prior to actuating NMR analysis of the observe volume in the microcoil.