Guiana dolphins produce whistles with a higher frequency and less complexity than most other delphinid species. The present study used a recording system with sampling rate of 192 kHz to describe the high-frequency whistles of Sotalia guianensis in Guanabara Bay, Rio de Janeiro. Eleven acoustic parameters (start, end, minimum, maximum, delta, center and peak frequency, duration, and frequency at 14, 12, and 34 of duration) were measured for all whistles. Whistles with a fundamental frequency up to 66.7 kHz were reported, thereby expanding the known frequency range of this species.