The aim of the article was the synthesis of novel l-phenylalanine derivatives with biological activity and their immobilization into polymeric particles. Thus, new formyl, acetyl and p-methoxy derivatives of l-phenylalanine with antitumor activity were synthesized by reaction with p-nitrobenzoyl chloride, followed by the reduction of nitro group and acylation of the new formed amino group. The chemical structures of the obtained aminoacid derivatives were determined by FT-IR, NMR, MS and elemental analyses. The compounds were encapsulated into chitosan- and gelatin-based submicronic capsules, prepared by double crosslinking (ionic and covalent) in a O/W/O double emulsion. The varying parameter polymer/ionic crosslinker molar ratio was seen to influence particle size, morphology, swelling degree, thermal properties, as well as their capacity to incorporate and release the new active principles. The in vivo acute toxicity and antitumoral effect of aminoacid derivatives in free form or encapsulated were evaluated on rats. Drug encapsulation into polymeric systems was proven to enhance antitumoral activity against implanted Guerin's carcinoma.