The objective of this study was to identify the main floral scents and their relative contents in the floral organ of Nelumbo nucifera. N. nucifera flower, a traditional Chinese medicinal herb, is rich in volatile compounds. In this study, the volatile components of N. nucifera flowers were investigated by headspace solid-phase microextraction gas chromatography-mass spectrometry for each organ of the flower: petals, sepals, pistils, and stamens. In total, we identified 39 compounds, among which aliphatics were major constituents, representing more than 94% of petals and sepals volatiles, followed by sesquiterpenes representing more than 69% of pistils and stamens volatiles. Pentadecane, 1-pentadecene, 8-hexadecyne, 8-heptadecene, and β-caryophyllene characterize the scent of the N. nucifera flower. We identified 24 volatiles in petals and sepals, 25 volatiles in pistils, and 18 volatiles in stamens. Among the monoterpenes, 3-Isopropylidene-4-methylcyclohexene, isoterpinolene, p-Menth-2-en-7-ol, and methyl 2,6,6- trimethylcyclohex-1-enecarboxylate were analyzed and identified for the first time from the N. nucifera flower. This study demonstrates that N. nucifera flowers differ greatly in volatile composition depending on the floral organ of the plant.