The volatile components of the Dufour's gland extracts ofDufourea novaeangliae were analyzed by gas chromatography-mass spectroscopy. The following were identified: a series of five bis-homologous unsaturated ketones ranging from C10 to C18, a series of nine bis-homologous hexanoates ranging from C8 to C24, a series of three bis-homologous octanoates ranging from C8 to C12, and hexanoic, hexadecanoic, and octadecanoic acids. The ketones are all new natural products reported for bees. Several of these unsaturated ketones were also identified in extracts of the provision masses from their nest cells. Male mandibular gland extracts contained citral.