Nitric oxide (NO) is the downstream effector after the activation of N-methyl- D-aspartate (NMDA) receptors. It is involved in various physiological processes, such as synapse reconstruction and plasticity, neurotoxity and neuronal death. It also participates in the development and maturation of cortical neurons. The expression of nitric oxide synthase (NOS) during the postnatal development of the visual cortex was investigated by both electron spin resonance (ESR) and Western blot methods. A typical spectrum of (DETC) 2-Fe(II)-NO complex was found in the visual cortex of different age golden hamsters by ESR method. The signal intensity increased after birth, peaked at postnatal day 14 (PD14) and then gradually decreased. An analysis of variance (ANOVA) implied that the NO synthase expression significantly correlated with the developmental processes ( p<0.05). Results of Western blot further confirmed (one-way ANOVA, p<0.05) the developmental relating expression pattern of NO synthase shown by ESR technique.