The synergistic effects of Cu, Fe, Mn, Zn, and Al on the evolution of different volatile sulfur compounds (VSCs) in a Chardonnay and a Shiraz wine have been investigated. The evolution of H2S, MeSH, and DMS were influenced by metal addition, and in some instances, a combination of metals was responsible for the largest variation in the concentration of VSCs. The metals and metal combinations associated with significant changes in VSC concentrations in both Chardonnay and Shiraz samples after anaerobic storage were Cu, Fe, Zn, Al, Cu*Fe, Cu*Mn*Al, and Cu*Zn*Al for H2S; Cu, Zn, Fe*Mn, and Cu*Fe*Mn for MeSH; and Al and Zn*Al for DMS. The effect of Cu addition on the evolution of VSCs has previously been shown; however, this investigation has demonstrated that metals other than Cu could also be involved in the catalytic release of VSCs and that the interactions and combinations of metals are important. In some instances, the metal effect was reversed, associated with significant decreases during high oxygen conditions and with significant increases during low oxygen conditions.