Xylan, a hemicelllulose extracted from corn cobs, was used to prepare micro and nanoparticles. First, a chemical evaluation of xylan extract was performed. Then, particles were prepared by a coacervation method based on neutralization of an alkaline solution with an acid solution. The influence of polymer content (2.85 to 100 mg/ml) and surfactant presence (0.6 to 1.8%((v/v))) on the manufacturing process was evaluated. It was demonstrated that neutralization of the xylan solution with HCl or acetic acid was able to generate micro and nanoparticles and that surfactant concentration influences both the particle size stability and morphology. Therefore, the: optimal concentration of surfactant was 1.5%((v/v)).