Volatile compounds are chemical species responsible for the distinctive aroma of virgin olive oil. Monovarietal olive oils have a peculiar composition of volatiles, some of which are varietal descriptors. In this paper, the total phenolic content (TPC), fatty acid composition, volatile compounds, and sensory profile of monovarietal olive oils from four Dalmatian most common olive cultivars—Oblica, Lastovka, Levantinka, and Krvavica—were studied. The volatile composition of olive oils was analyzed using headspace solid-phase microextraction with gas chromatography/mass spectrometry. The highest mean TPC value was measured in Oblica and Krvavica oils (around 438 mg/kg). The difference among cultivars for fatty acids composition was detected for C16:1, C17:0, C18:1, C18:2, and the ratio C18:1/C18:2. Krvavica oils showed clear differences in fatty acid composition compared to oils from other cultivars. The most prevalent volatile compound in all oils was C6 aldehyde E-2-hexenal, with the highest value detected in Levantinka oils (75.89%), followed by Lastovka (55.27%) and Oblica (54.86%). Oblica oils had the highest value of Z-3-hexen-1-ol, which influenced its characteristic banana fruitiness, detected only in this oil. Lastovka oils had the highest amount of several volatiles (heptanal, Z-2-heptenal, hexanal, hexyl acetate), with a unique woody sensation and the highest astringency among all studied cultivars. Levantinka oils had the highest level of almond fruitiness, while Krvavica oils had the highest level of grass fruitiness.
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