Two barley varieties, Gan4 and Hamelin, were malted to investigate the evolution of phenolic compounds and antioxidant activity during malting. The antioxidant activity was evaluated with DPPH radical scavenging activity, ABTS radical cation scavenging activity, reducing power, and metal chelating activity. Results showed that malting had significant influences on individual and total phenolic contents as well as antioxidant activities of two barley varieties. The contents of some phenolic compounds and the antioxidant activities decreased significantly during steeping and the early stages of germination and then increased remarkably during the later stages of germination and subsequent kilning. The most phenolic compounds identified in barley were (+)-catechin and ferulic acid, which both changed significantly during malting. Moreover, results from the Pearson correlation analysis showed that there were good correlations among DPPH radical scavenging activity, ABTS radical cation scavenging activity, reducing power, total phenolic content and sum of individual phenolic contents during malting.