Analysis of Volatile Organic Compounds (VOCs) in crude coconut and petroleum oils from Nigeria is reported. Using head-space gas chromatography with a flame ionization detector and mass spectrometer, 8 VOCs were found in crude coconut oil and 29 VOCs were identified in crude petroleum oil. Crude coconut oil contained two aromatic, two nitrogenated, and four oxygenated compounds. Alkane, alkene, alkyne, halogenated, and sulfur compounds were absent in crude coconut oil but not in crude petroleum oil. The same observation held true for naphthalene. Conversely, benzofuran was absent in crude petroleum oil but was present in crude coconut oil at a concentration of 1.38 part-per-billion (ppb). The most concentrated VOC in crude coconut oil was dodecanoic acid at 9.98 ppb and that of crude petroleum oil was toluene at 12.61 ppb. Total VOC concentrations in crude coconut and petroleum oils are 20.49 and 87.46 ppb, respectively. These results are helpful in characterizing the chemical signature of Nigerian crude coconut oil for potential forensics use or in biofuel research.