The ripe fruits of Maclura tricuspidata (formerly Cudrania tricuspidata) are bright red in color and are edible with a floral aroma and sweet taste. They have traditionally been used to prepare fresh juice, jam, wine, vinegar and alcoholic beverages in Korea. This study was carried out to characterize the volatile aroma components of wine and vinegar prepared from M. tricuspidata fruit by yeast (Fermivin) and Acetobacter pasterianus YJ17. Its volatile aroma components were also compared with those of six commercial vinegars (three domestic vinegars and three foreign balsamic vinegar products). Volatile compounds were separated by solid-phase extraction (SPE) using Amberlite XAD-2 as a sorbent. Fifty-seven compounds, including 15 alcohols, 15 esters, 12 aldehydes and ketones, 7 acids and 8 miscellaneous compounds were identified by gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) analyses in the seven vinegars and the M. tricuspidata wine sample. The newly prepared M. tricuspidata fruit vinegar (MTFV) contained 47 of them. Among all the identified compounds, ethyl hydrogen succinate, phenylacetic acid, p-hydroxybenzyl alcohol, p-hydroxybenzaldehyde, p-hydroxyphenylacetic acid, tyrosol (p-hydroxyphenylethyl alcohol), dihydroactinidiolide, 3-hydroxy-β-ionone and tryptophol were only detected in the MTFV. p-Hydroxybenzyl alcohol, p-hydroxybenzaldehyde, p-hydroxyphenylacetic acid and tyrosol have been reported to have various biological activities. Therefore, their exclusive presence in the MTFV may contribute to its health benefits.