This study applied the macromonomers and glycidyl methacrylate (GMA) to synthesize a series of the graft copolymers, poly(GMA)-graft-poly(Z-L-lysine), and investigated the conformation of the graft copolymer. The graft copolymers were synthesized with different GMA monomer ratios (28 to 89%) and different degrees of polymerization (DR) (8 to 15) of the poly(Z-L-lysine) side chain to analyze secondary structure relationships. Atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FTIR), and both wide angle and small angle X-ray scattering spectroscopy (WAXS, SAXS) were used to investigate the relationship between the microstructure and conformation of the graft copolymers and the different monomer ratios and side chain DR In AFM images, n8-G89 (the graft copolymer containing 89% GMA units and the macromonomer DR is 8) showed tiny and uniform rod-like structures, and n14-G43 (the graft copolymer containing 43% GMA units and the macromonomer DP is 14) showed uniform rod-like structures. FTIR spectra of the graft copolymers showed that the variations of alpha-helix and beta-sheet secondary structures in the graft copolymers relate to the monomer ratios of the graft copolymers. However, the X-ray scattering patterns indicated that the graft copolymer conformations were mainly dependent on the poly(Z-L-lysine) side chain length, and these results were completely in accordance with the AFM images. (C) 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 47: 4655-4669, 2009