The experimental verification of offset profiles and calibration of selecti
ve pulses in NMR is usually carried out with doped water samples but not un
der conditions typical of macromolecules with short T-2, long T-1, and poss
ibly homo- and heteronuclear couplings. A new method for selective excitati
on in isotopically labeled macromolecules is shown to be particularly suite
d to this purpose. This is illustrated for a backbone amide resonance in a
sample of N-15-labeled human ubiquitin, (C) 1999 Academic Press.