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Black garlic is popular as food supplement as well as herbal medicine due to its rich and beneficial chemical content. The chemical changes during the process are rarely investigated. The purpose of the study was to determine the effect of heating time on sulfur-containing compounds profiles and antioxidant activity during fermentation process at 60oC. The process is followed by GC-MS and the antioxidant activity was seen using DPPH. The result indicates that black garlic undergoes changes of sulfur-containing organic secondary metabolites, such as allicin and its related compounds. This process also reduces the percentage of black garlic inhibition, which increases the antioxidant activity of black garlic, and shows that black garlic contains very good antioxidant compounds.