Nitric oxide (NO) plays an important role in biology as a mediator, for example, of the endothelial-derived relaxing factor (EDRF)Ðan agent responsible for the regulation of blood vessel relaxation and for the maintenance of blood pressure. [1] Concentrations of 30 to 300 ppm of NO (1 ppm % 3.3 Â 10 À5 m) are sufficient to activate the guanylyl cyclase signaling cascade. [2] Since NO is a gaseous and highly reactive species, its direct detection at low concentrations is difficult. The methods used to sense NO have generally been based on following changes in the UV/Vis spectra or electrochemical properties of the sensing elements. [3] Electron paramagnetic resonance (EPR) and NMR image visualization of the distributions of NO free radicals in vivo were also reported, but were found to be limited by spatial resolution and sample size. [4,5] We report here a novel approach for the direct detection of low concentrations of NO free radicals in physiological aqueous solution (pH 7.4).The Molecular Controlled Semiconductor Resistor (MOCSER; see reference [6]) provides an excellent way toThe use of this spin-trap for the in vivo detection of NO is more problematic because of the presence of reducing agents: when 2 was treated with ascorbic acid and the reaction monitored by EPR spectrocopy, the typical spectrum of 9 e (Scheme 2 where X OH, Y 1 Y 2 H) immediately appeared and then decayed, but, as expected, at a much lower rate. [8] However, it is possible to distinguish between the NO adducts and 9 e by combining different analytical methods such as mass spectrometry, 1 H NMR spectroscopy, [7] (for 9 a and 9 b) and probably by high-field EPR spectroscopy. [15] Analogously other spin-labeled spin-traps may be used to study the reactions of a radical R T with reactive radicals. [16]