Polycyclic Aromatic Hydrocarbon (PAHs) Analyses in Marine Tissues Using Accelerated Solvent Extraction (ASE) in Tandem with In-Cell Purification and GC MS

The aim of this research was the replacement of conventional sample extraction techniques for polycyclic aromatic hydrocarbons (PAH) in tissue samples for a reliable, fast and eco-friendly procedure. The method was developed using a pressurized solvent extraction method and assessing two different standard reference materials (fish and mussel) and freeze-dried and fortified sardine samples (Sardinella sp.). Five different extraction procedures were evaluated and the best performance comprised 1 g of lyophilized tissue, 5 g of deactivated (5%) silica, a dichloromethane:methanol (4:1 v/v) mixture, a temperature of 80 °C, three cycles, 10 min of static time and 90 s of purge time. The method selected following these tests was further validated through the analysis of nine replicates of the National Institute of Standard and Technology (NIST) reference material No. 2976, resulting in an effective recovery of 83 ± 14%. The means and uncertainties attained for each PAH were equivalent to those of the reference material, corroborating the reliability of the developed method. A shorter processing time, less use of solvents and reagents and lower extract manipulation produced an effective method aligned with green-chemistry guidelines.

Keywords:
PAH analysis; tissue samples; method development; accelerated solvent extraction; green chemistry