GC-MS analysis of the metatarsal gland secretion from a female sika deer, Cervus nippon, showed 35 major volatile compounds that included 13 straight-chain carboxylic acids, a single branched-chain carboxylic acid, 9 straight-chain aldehydes, 3 monounsaturated aldehydes, 5 long-chain alcohols, a ketone, and cholesterol. The four most abundant compounds were heptanal, nonanal, octanoic acid, and 6-methyl-2-heptanone. Many of the compounds have previously been found in cervid secretions, but the unsaturated aldehydes, (E)-2-octenal, (E)-2-nonenal, and (E)-2-decenal, have not previously been reported in the glands of any cervid. The compounds in this gland may be pheromones, since metatarsal gland odor has been implicated in chemical communication among conspecifics of other cervids.