Confocal Raman spectroscopy was undertaken to identify separate layers of PLGA and gentamicin sulfate (GS) coatings on a titanium alloy substrate for a novel drug-delivery system. Additionally, it was found that it was possible to measure the layer thickness and uniformity of the PLGA accurately by detecting intensity and wavelength changes in the vibrational bands of the copolymer bonds. Further analysis of the materials was done using FIB, SEM/EDX, and profilometry; these techniques were used to confirm the findings of the Raman data. It was determined that the substrate was extremely rough and therefore the coating was not uniform in thickness but the materials were uniformly dispersed. Most importantly, two distinct GS and PLGA layers were present.