The composition of bitter orange petitgrain oil was studied by HPLC-GC/MS (ITD) and GC/MS (quadrupole), and it was found that data obtained with the two methods were in good agreement. The LC-GC system allowed the LC separation of the oil into two fractions (hydrocarbon and oxygenated compounds), then the automated transfer in GC prior to the identification of the components. Bitter orange petitgrain oil showed a high content of oxygenated compounds which varied from 91% to 96%. Linalyl acetate, which represented more than 50% of the whole oil, and linalool, which ranged from 22% to 33%, were the main components. Limonene, (E)-β-ocimene, myrcene and β-pinene were the highest monoterpene hydrocarbons. Twelve sesquiterpene hydrocarbons were identified. β-Caryophyllene is the most representative of this fraction.