Optimized simultaneous pressurized fluid extraction and in-cell clean-up, and analysis of polycyclic aromatic hydrocarbons (PAHs), and nitro-, carbonyl-, hydroxy -PAHs in solid particles

The development, modification and optimization of analytical methods capable of simultaneous extraction and in-cell clean-up of extracts for subsequent determination of parent PAHs and their associated transformed nitro-PAHs (NPAH), carbonyl-PAHs (CPAH) and hydroxy-PAHs (HO-PAH) products (TPPs) is essential for reducing the time and cost of analysis. The aim of this study was to modify and optimize the pressurized fluid extraction (PFE) technique capable of simultaneous extraction and in-cell clean-up of PAHs and TPPs in urban dust standard reference material and road dust for GC-MS analyses. In this study, multivariate data analysis such as factor analysis (FA), and preference ranking organisation method for enrichment evaluation (PROMETHEE) and geometrical analysis for interactive aid (GAIA) were used to assess the performance of the methods. As the key outcome of the study, an optimized selective reaction monitoring (SRM) Triple Quadrupole (TQ) electron ionization (EI)-GC/MS for measuring PAHs and TPPs without derivatization of polar HO-PAHs was developed. The limits of detection (LOD) for parent PAHs, CPAHs, NPAHs and HO-PAHs using Shimadzu TQ were 1.0–5.0 pg, 1.0–5.0 pg, 1.0–50.0 pg, and 1.0–25.0 pg, respectively. The PROMETHEE-GAIA analysis of the results showed that a combination of 3% deactivated silica gel and activated alumina (2:1) as in-cell clean-up material, and sequential PFE extraction (200 °C ASE temperature, 9 min preheat time and 3 times extraction cycle) using 100% hexane followed by hexane/DCM (1:1) is the best condition for analytes extraction from road dust. An optimized, fast and reliable GC/MS method operated solely in electron ionization (EI) mode was developed for measuring all analytes. The outcomes of this study will contribute significantly to future research on PAHs and TPPs, thereby promoting a safe and sustainable environment.