Coaxial electrospray is an emerging technology to produce multilayer micro- and nano-particles (NPs) with well controlled shape and size. ALA-PDT is a fascinating technology used in the treatment for skin and other cancers. In this work, ALA-loaded poly(lactide-co-glycolide) (PLGA) (PLGA-ALA) NPs with high drug loading efficiency were produced via coaxial electrospray and used for the PDT treatment in HSC-3 cells.