Trichosporins are a linear peptide mixture produced by Trichoderma polysporum whose structures are closely similar to each other. They inhibits the growth of Lentinus edodes. These peptides belong to peptaibols in which the N-terminal is protected by an acetyl group and the C-terminal by a phenylalaninol. Recently, we have isolated trichosporins[TS]-B-IIIb(1), c(2), IVb(3), c(4), d(5) and VIa(6), b(7) and established their primary structures by positive ion FAB-MS spectrometry, respectively. TS-B-IVb,d and VIb are the first examples of isovaline containing peptides isolated from T. polysporum. The connectivities of amino acid residues are established by means of COSY and NOESY NMR techniques. In addition, uncoupling activities of these peptides on rat liver mitochondria were examined.