A new chemical synthesis has been disclosed for the oxidizing and nitrating species peroxynitrite. This nitric oxide and superoxide-derived cell signaling mediator can also serve as a toxicant at higher rates of generation. The new synthetic strategy reported by Sturzbecher-Höhne and colleagues overcomes long-standing issues with purity and quality of peroxynitrite preparations and should lay a foundation for nailing new insight into the redox reactions of peroxynitrite and its products.