We present a new technique for double-quantum excitation in magic-angle-spi
nning solid-state NMR, The method involves (i) preparation of nonequilibriu
m longitudinal magnetization; (ii) mechanical excitation of zero-quantum co
herence by spinning the sample at rotational resonance, and (iii) phase-coh
erent conversion of the zero-quantum coherence into double-quantum coherenc
e by frequency-selective spin inversion. The double-quantum coherence is co
nverted into observable magnetization by reversing the excitation process,
followed by a pi/2 pulse. The method is technically simple, does not requir
e strong RF fields, and is feasible at high spinning frequencies. In [C-13(
2),N-15]-glycine, with an internuclear C-13-C-13 distance of 0.153 nm, we a
chieve a double-quantum filtering efficiency of similar or equal to 56%. In
[11,20-C-13(2)]-all-E-retinal, with an internuclear C-13-C-13 distance of
0.296 mn, we obtain similar or equal to 45% double-quantum filtering effici
ency. (C) 2000 Academic Press.