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Summary: Nanocapsules were prepared by interfacial polycondensation of an oil-soluble monomer (phthaloylchloride) and a hydrophilic monomer (diethylentriamine). Upon addition of the oil phase to the aqueous phase, interfacial reaction takes place at the interface of an oil in water submicronic emulsion. After the initial formation of the wall, the polycondensation is diffusion controlled. The influence of different variables on nanocapsules size was evaluated. Oil (Miglyol® 812) concentration played an important role by controlling the size of the emulsified droplets (precursor of nanocapsules). Ratio of lipohilic to hydrophilic monomer showed a significant effect on the size, indicating that polymeric walls of difference thicknesses can be obtained. The introduction of a lipohilic surfactant (Lipoid® S75) and a hydrophilic surfactant (Pluronic®F68) in the formulation is important for the stability of nanocapsules after their preparation.