The essential oils from two members of the Asteraceae ( Acanthospermum hispidum DC. aerial parts, and leaves of Tithonia diversifolia (Hemsley) A. Gray), growing wild in Osun State, Nigeria, have been characterised by combined gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) analyses. Twenty-nine components have been fully identified and grouped into monoterpene hydrocarbons (22.2%), oxygenated monoterpenes (4.6%), sesquiterpenes hydrocarbons (58.2%) and oxygenated sesquiterpenes (10.8%) in A. hispidum. The main constituents of the oil were β-caryophyllene (28.0%), α-pinene (15.9%) and bicyclogermacrene (11.0%) among the hydrocarbon compounds, and bisabolol (8.9%) and carvacrol methyl ether (4.1%) among the oxygenated components. Tithonia diversifolia essential oil comprised seventeen components and was characterised by a predominant content of monoterpene hydrocarbons (87.9%), cis-β-ocimene (43.7%), α-pinene (28.6%) and limonene (12.0%) being the main compounds. Sesquiterpenes represented ca. 10% oil, as sum of hydrocarbons and oxygenated components. A new chemotype is established for T. diversifolia, while the Nigerian A. hispidum is being reported for the first time as a new source of essential oil with some distinction in composition from those of other sources.