Deuterium-labeled 5-oxo-Pro-Arg-Pro, 5-oxo-Pro-His-Pro-Gly-Pro-NH 2 , and Phe-Pro-LeuPro-Ala were synthesized. The effect of the method of peptide deposition on the catalyst, the catalyst nature, temperature, and structure of peptides on the inclusion of deuterium with the formation of the appropriate number of isotopomers was demonstrated. The 5-oxo-Pro-Arg-Pro, 5-oxo-Pro-His-Pro-Gly-Pro-NH 2 , and Phe-Pro-Leu-Pro-Ala peptides containing, on average, 4.6, 7.7, and 5.4 deuterium atoms per peptide molecule, respectively, were obtained.