In the current study, sediment samples from Zwitina Harbor in northeastern Libya were analyzed using a GC-Mass apparatus. The objective was to evaluate how the region's activities related to petroleum use affected the environment. The findings indicated the existence of several hydrocarbon compounds that might have an impact on marine life. Numerous aromatic compounds and aliphatic hydrocarbons (C9 to C20) were found. Several polyaromatic hydrocarbons were detected, including Benzo(g, h, i) perylene, Acenaphthylene, Fluorene, Phenanthrene, Anthracene, Pyrene, Benzo(a)anthracene, Chrysene, Benzo(b)fluoranthene, Benzo(k)fluoranthene, Benzo(a)Pyrene, Indeno(1,2,3-cd)pyrene, and Dibenzo(a,b)anthracene. The study deduced that sediment samples showed the effects of activities related to the petroleum sector and that the majority of petroleum compounds in the area come from pyrolytic and petrogenic sources.