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Volatile oils were extracted from aqueous leaf suspensions of sweet orange [Citrus sinensis (L.) Osb.] cultivars Hamlin, Navel, and Valencia and grapefruit (Citrus paradisi Macf.) cultivars Marsh and Ray Ruby. Pressurized air was used as the sparging gas, and volatile oils were collected in a C-18 cartridge. Gas-liquid chromatography was used to separate and quantify 17 volatile components. Significant quantitative differences for individual components made it possible to distinguish sweet orange from grapefruit (four components), `Marsh' from `Ray Ruby' grapefruit (two components), `Hamlin' from `Valencia' or `Navel' orange (six components), and `Valencia' from `Navel' (three components). The simplicity and sensitivity of the procedure suggest potential use for Citrus taxonomic, genetic, and breeding research.