In this study we demonstrate formation of nitric oxide in aqueous nitrogen-containing solutions exposed to 50 kHz cavitation-producing ultrasound (standard bath sonicator) using electron paramagnetic resonance detection of • NO by trapping with the sodium N-methyl-D-glucamine dithiocarbamate iron(II) complex ((MGD) 2 Fe 2+ ) or by measuring the conversion of the nitronyl nitroxide, 2-(4-carboxyphenyl)-4,4,5,5-tetramethylimidazoline-3-oxide-1-oxyl (carboxy-PTIO), to the imino nitroxide, 2-(4-carboxyphenyl)-4,4,5,5-tetramethylimidazoline-1-oxyl. The (MGD) 2 Fe 2+ complex which was used in most experiments was suitable for • NO detection over a wide pH range (pH 3-7.8; the working range for carboxy-PTIO was pH 6-8.5), and the measured rate constant of (MGD) 2 Fe 2+ reaction with • NO was 2.3 times higher than for carboxy-PTIO. In air-saturated water the rate of • NO production by ultrasound was ∼0.5 µM/min. The presence of dissolved oxygen was not essential for production of • NO; the highest yields of • NO (∼1.2 µM • NO/min) were found under an atmosphere of 40% N 2 and 60% argon. The formation of • NO by ultrasound in aqueous solutions can be understood in terms of combustion chemistry-type reactions occurring inside the "hot" collapsing cavitation bubbles. We also show that other N-containing molecules can serve as a source of nitrogen for • NO production. The possibility of ultrasound-mediated • NO formation to alleviate hypoxia of tumors should be explored.