Annotation.The paper presents the results of experiments on the application of the method of optical emission spectroscopy of a glow discharge for the profile analysis of vacuum-deposited single and two-layer films of multicomponent garnet ferrites of various compositions before and after crystallization annealing. The presence of internal and external transition layers was revealed, and the modification of their elemental composition during crystallization, as well as the different sequence of synthesis of individual components in ferrite-garnet heterostructures, was investigated.