Polycyclic aromatic hydrocarbons (PAHs) are highly persistent, hazardous (cause cancer), and widespread pollutants. Their presence in the environment is a public health concern. Identifying and determining these PAHs are first step in developing measures for the removal of these compounds from water and sediment. The aim of this study was to compare and optimize three different extraction methods for the detection of PAHs in sediment samples. The optimized methods include microwave assisted extraction (MAE), ultrasonication (U), and a combination of ultrasonication and mechanical shaking (UAM). PAHs in the certified reference material of sediment (CRM-104) were quantified to confirm the accuracy of the proposed methods. Gas chromatography coupled with flame ionization detector (GC-FID) was used for analysis of 16 PAHs. Due to its superior precision compared to ultrasonication and combined ultrasonication and mechanical shaking, which both displayed subpar precision, the MAE was preferred for the extraction of PAHs from sediment. Furthermore, the MAE was found to be the most versatile technique due to its easy handling and fast extraction time when many samples are analysed; also, it implies low operation costs. The MAE was successfully applied in determining the concentrations of 16 PAHs in real sediment samples with good precision and excellent percentage recoveries (between 83.8 and 125%). The concentrations of PAHs obtained using the three extraction methods ranged between 0.016 and 10.8 mg/kg. In general, lower molecular weight compounds showed lower concentration than higher molecular weight PAHs, and the values displayed spatial variation.