Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)A new technique using diffuse reflectance spectroscopy was developed that enables the monitoring of encapsulated drug release without particle separation from the assayed medium. Studies of chloro(5,10,15,20-tetraphenylporphyrinato)indium(III) (InTPP) release from microspheres and nanospheres of poly(lactide-co-glycolide) (PLGA) were performed using this new technique. The release of InTPP was biphasic, with an initial fast release followed by a second slower release. Mathematical models applied to the release profiles showed that the release of InTPP from the nanospheres was controlled by diffusion, which is to be expected for a substance homogeneously dispersed within the spheres. However, due to the large size distribution of the microspheres loaded with InTPP, the release profiles were irregular, hampering an adequate fit to mathematical models. Confocal analysis of microparticles showed that the InTPP appeared to be homogenously distributed within the microspheres and no preferential distribution of InTPP towards the interior or towards the surface of the spheres was observed.212214225Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Universidade Estadual de CampinasFundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)