Two techniques for resolution and sensitivity enhancement are introduc
ed in multiple-quantum (MQ) MAS spectroscopy of rigid solids. The firs
t makes use of ultrafast MAS with spinning frequencies of up to 35 kHz
, while the second combines MAS at moderately fast spinning frequencie
s of about 13 kHz with multiple-pulse (MP) dipolar decoupling. For the
latter approach, a semiwindowless WHH-4 sequence is applied during th
e MQ evolution period (MQ dimension) and/or detection period (single-q
uantum dimension). In the MQ dimension, the MP sequence has to be supp
lemented by two bracketing pulses in order to preserve the order and t
he intensities of the evolving MQ coherences. Double-quantum H-1 NMR s
pectra of L-alanine recorded using both decoupling techniques are show
n and compared to each other. Triple-quantum H-1 NMR spectra under ult
rafast MAS conditions are also presented, (C) 1998 Academic Press.