The method of depth profiling of low temperature photoluminescence spectra was applied to the study of samples GaP: Zn, O prepared by LPE technology. The obtained results were used to calculate the depth profiles of zinc and sulphur concentration in the samples. Several layers showed considerable variations of the red emission band shape with the depth of measured region (atT ≈ 85 K) due to the changes in mutual intensity ratio of several bands lying in this spectral region. Primarily the bands corresponding to exciton and pair mechanism of radiative recombination on the complexes (O-Zn) and a shortwave emission band with the peak near the energy of 1·89 eV are concerned.