Most frequently arsenic is nominally monovalent (As 1-) in pyrite (FeS2) and substituted for S. Nominally trivalent arsenic (As 3+) has been reported previously in hydrothermal Peruvian pyrite and was considered to be substituted for Fe based on the negative correlation between the concentrations of the two elements. Here, we provide the first observation of the incorporation of As 3+ in goldfieldite (Cu12(As,Sb,Bi)2Te2S13) and As 5+ in colusite (Cu26V2(As,Sb)4Sn2S32) inclusions in As 1-pyrite from high-sulfidation deposits in Peru. This information was obtained by combining spatially-resolved electron probe (EPMA), synchrotron-based X-ray fluorescence (SXRF) and absorption spectroscopy (micro-XANES and micro-EXAFS) with new high energy-resolution XANES spectroscopy (HR-XANES). The two Cu sulfide inclusions range from several to one hundred micrometers in size and the As 3+ /As 5+ concentration varies from a few parts-per-million (ppm) to a maximum of 17.33 wt%, compared to a maximum of 50 ppm As 1in pyrite. They also contain variable amounts of Sn (18.47 wt% max.), Te (15.91 wt% max.), Sb (8.54 wt% max.), Bi (5.53 wt% max.), and V (3.25 wt% max.). The occurrence of As 3+ /As 5+-containing sulfosalts in As 1-containing pyrite grains indicates that oxidizing hydrothermal conditions prevailed during the late stage of the mineralization process in the ore deposits from Peru.