Lemon [Citrus limon (L.) Burm. f.] and grapefruit (Citrus paradisi Macf.) peel oils were obtained by cold-pressing lemon and grapefruit peels. The oils were analyzed by high-resolution gas chromatograph (HRGC) and high-resolution gas chromatography/mass spectrometer (HRGC/MS). In total, 42 and 27 components have been identified in lemon and grapefruit oils, respectively. Lemon oil showed a high content of monoterpene hydrocarbons (89.9%) with limonene (61.8%),,gamma-terpinene (10.6%) and beta-pinene (8.1%) being the first three major components. Similarly, grapefruit oil was characterized by its higher content of monoterpene hydrocarbons (96.4%) of which limonene (92.5%) and myrcene (2.6%) were the first two major components. Grapefruit oil contained a lower amount of sesquiterpene hydrocarbons, aldehydes, alcohols and esters than that in lemon oil.