Previous studies suggested the presence of desglycyl peptides in Cd-peptide complexes of Schizosaccharomyces pombe and other fungi via amino acid composition analysis. In this study, the peptides in a Cd-peptide complex of S. pombe were characterized using FRIT-FAB LC/MS, a coupling technique of high-performance liquid chromatography (HPLC) with fast atom bombardment mass spectrometry. S. pombe was cultured in a medium containing 1 mM CdCl₂ for 6 days. The cells were harvested, homogenized, and the supernatant was purified via Sephadex G-50 gel filtration and QAE-Sephadex A-25 ion exchange chromatography. FRIT-FAB LC/MS analysis of the purified Cd-peptide complex identified four peptide peaks (P-1 to P-4): P-1 was (γ-Glu-Cys)₂-Gly, P-2 was desglycyl (γ-Glu-Cys)₂, P-3 was (γ-Glu-Cys)₃-Gly, and P-4 was desglycyl (γ-Glu-Cys)₃. The levels of desglycyl peptides increased with culturing period. These desglycyl peptides can form heavy metal complexes and may function in heavy metal detoxification together with (γ-Glu-Cys)ₙ-Gly (n ≥ 2). The synthetic mechanisms of desglycyl peptides (e.g., transfer of γ-Glu-Cys moiety or hydrolytic cleavage of Gly by carboxypeptidase) remain unclear and require further investigation.