Hydrogels are materials composed mostly of water that have found use in a wide variety of applications, including tissue engineering and regenerative medicine. Aromatic peptide amphiphiles can be designed to self-assemble in aqueous solution into one-dimensional aggregates that entangle to form hydrogels with very high water content (>99 wt. %). Here, we describe the synthesis of an aromatic peptide amphiphile designed to release hydrogen sulfide (HS), a vital biological signaling gas with significant therapeutic potential. Peptide synthesis, purification, aliquotting, and procedures for measuring HS release are detailed.