Concentrations of tetrabromobisphenol A (TBBPA) and alpha-, beta-, and gamma-isomers of hexabromocyclododecanes (HBCDs) were determined by liquid chromatography-tandem mass spectrometry (LC-ESI-MS/MS) in human adipose tissue obtained in New York City, and in three marine top-level predators--bottlenose dolphin, bull shark, and Atlantic sharpnose shark--collected from coastal waters of Florida, USA. The overall mean concentrations (mean+/-SD) of TBBPA and HBCDs were 0.048+/-0.102 and 0.333+/-0.571 ng/g lipid wt in human adipose tissue samples, 1.2+/-3 and 7.38+/-18 ng/g lipid wt in bottlenose dolphin blubber, 9.5+/-12 and 77.7+/-128 ng/g lipid wt in bull shark muscle, and 0.872+/-0.5 and 54.5+/-88 ng/g lipid wt in Atlantic sharpnose shark muscle. Overall mean concentrations of HBCDs were 5-10-fold higher than mean TBBPA concentrations, in all of the samples analyzed. The highest concentrations of TBBPA and HBCDs were detected in the bull shark muscle at concentrations of 35.6 and 413 ng/g, lipid wt, respectively. Concentrations of TBBPA and HBCDs, after log-transformation, were significantly correlated with each other in human adipose tissue and bottlenose dolphin blubber, but not in bull shark muscle samples. In the human adipose tissue samples, the concentrations of HBCDs were 3-4 orders of magnitude lower than the concentrations of polybrominated diphenyl ethers (PBDEs) previously reported for the same set of tissue samples. Concentrations of HBCDs in human samples from the United States were 1-5-fold lower than the concentrations reported from several European countries. HBCD concentrations in bottlenose dolphins from the United States were 1-2 orders of magnitude lower than the concentrations reported for other cetacean species from Europe. The present report is the first to determine levels of TBBPA and HBCDs in humans, bottlenose dolphins, and sharks from the United States.