Volatile oils from leaf and stem of Calotropis procera Ait, an Asclepiadeae were analyzed for their constituents by means of gas chromatography and gas chromatography coupled with mass spectrometry. Nine compounds were identified in leaf, and ten in stem, which are respectively responsible for 93.9% and 86.4% of leaf and stem oils. Leaf oil is dominated by tyranton (54.4%), 1- pentadecene (9.5%) and 1-heptadecene (8.2%). Most abundant compounds in stem oil are Z-13-docosenamide (31.8%), isobutyl nonane (13.7%) and 2,7,10-trimethyldodecane (12.3%). Both leaf and stem volatile oils contain octadecenamide and its saturated form in appreciable amounts. Also characteristic of these oils are the presence of long chain fatty acids and amides, sulfurate, halogen compounds and carbonyls like ketones. Chemical composition of Calotropis procera essential oil is reported for the first time in literature.