The superoxide scavenging activity of dihydrolipoic acid and its analogues has been reevaluated by a chemiluminescence method using MCLA as a superoxide indicator. The results demonstrated that all the compounds having the thiol chromophore in the molecule showed scavenging activity toward superoxide. The short-chain analogue, tetranor-dihydrolipoic acid, showed almost the same scavenging activity as that of dihydrolipoic acid; however, bisnor-dihydrolipoic acid showed weaker scavenging activity than that of dihydrolipoic acid. The reaction rates of dihydrolipoic acid, bisnor-dihydrolipoic acid, and tetranor-dihydrolipoic acid were calculated from the competitive inhibition of MCLA-superoxide reaction. Thus, it was concluded that dihydrolipoic acid and the analogues are good scavengers of superoxide radical anion.