The effects of different nuruk contents and fermentation methods (AV, vinegar fermented in an agitated culture; SV, vinegar fermented in a static culture) on organic acids and volatile compounds in brown rice vinegars were investigated. In the SV, the contents of acetic, oxalic, tartaric, and malic acids increased with hipher contents of nuruk. Acetic, tartaric, and malic acid contents were higher in the SV than those in the AV. Volatile compounds that can affect vinegar quality, including acetic acid, isoamyl acetate, phenethyl acetate, and phenethyl alcohol were present at high concentrations in the AV. With the increase in nuruk contents in the AV, acetic acid content decreased and isoamyl acetate and phenethyl acetate content increased. No significant differences in sensory scores were observed regarding the amount of nuruk and the type of fermentation. However, electronic-nose analysis showed its potential to effectively differentiate different samples.