Direct thermal desorption-gas chromatography-tandem mass spectrometry versus microwave assisted extraction and GC-MS for the simultaneous analysis of polyaromatic hydrocarbons (PAHs, PCBs) from sediments

Abstract

Polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs) are regulated contaminants usually investigated in sediments. Conventional approaches often use GC-MS to analyse them with a preliminary extraction step which can be solvent- and time-consuming. Here two extraction methodologies were optimized using experimental designs, and compared: microwave assisted extraction (MAE) and thermal desorption (TD); the latter was rarely used for sediments analyses. Several factors that may influence extraction recoveries were studied including matrix parameters (mass, organic matter (OM) content) and processing parameters. A definitive screening design DSD was performed to screen the 6 most influencing factors and model the extraction recoveries using TD. Whatever the OM content, a minimum sediment mass (5 mg) was better for an optimal extraction, with a minimum temperature rate (15 °C min−1), a maximum final temperature (350 °C) associated with a minimum hold time (5 min), and a maximum vent flow (150 mL min−1) between the TD unit and the cryogenic trap. Thereafter matrix effects were evaluated using standard addition, and quality assurance and control were implemented for comparing MAE and TD. TD-GC-MS/MS sensitivity was higher than MAE-GC-MS with detection limits in the range 5–1160 pg and 20–125 pg for PAHs and PCBs, respectively. When considering the appropriate strategy for quantification, TD was also reliable for sediments analysis. Although MAE was less sensitive to matrix effects, TD could significantly improve the analytical process, due to direct coupling with GC-MS/MS and complete automation. Moreover, TD offered possible higher spatial resolution than MAE, particularly for sediment cores analysis, due to the 1000-times lower sample size. At last, TD-GC-MS/MS appeared as a greener analytical procedure.