Pressurized hot water extraction coupled to solid-phase microextraction–gas chromatography–mass spectrometry for the analysis of polycyclic aromatic hydrocarbons in sediments

A fully automated, environmentally friendly, simple, and sensitive method was developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) in sediment samples. The procedure is based on pressurized hot water extraction (PHWE) followed by solid-phase microextraction (SPME) and determination by gas chromatography–mass spectrometry. For PHWE, parameters such as organic modifier, percentage of organic modifier, temperature, and static extraction time were studied. For SPME, extraction temperature and time, desorption temperature and time, splitless time, ionic strength adjustments, and effect of an organic modifier were studied. When these parameters were selected, the figures of merit were calculated. The detection and quantification limits were between 0.4–15 μg kg−1 and 1.2–51 μg kg−1, respectively. The linearity of the method was assessed spiking sediment samples at seven levels of concentration ranged between 2.5 μg kg−1 and 500 μg kg−1 for most of the studied PAHs. The method was validated by two concentration levels reference marine sediment materials (SRM 1944 and SRM 1941b). The obtained results are in very good agreement with the certificate materials. The developed method seems to be suitable for the analysis of PAHs at ultratrace levels in environmental matrices as sediment samples.