Zinc oxide (ZnO) and organophilic Clay (Viscogel B8) were added to poly(3-hydroxid butyrate) (PHB) matrix in some proportions. The nanocomposites containing both nanoparticles were obtained from solution casting method using chloroform as solvent. The films obtained were mainly analyzed by time-domain nuclear magnetic resonance (TD-NMR) to obtain answers about the interactions, dispersion, distribution of nanoparticles and, consequently, the homogeneity of both nanoparticles in the polymer matrix. Combining relaxation data of 1H measured at 23 MHz and from the longitudinal relaxation dispersions measured among 100 KHz to 300 MHz, it was also obtaining information on the influence of both nanoparticles in the polymer characteristics and if there was a synergic effect of ZnO nanoparticle and organoclay, using them together. The results obtained showed that the incorporation of only 0.1% of ZnO caused a great impact in the polymer PHB matrix and in the system obtained.