Determination of atmospheric particle-bound polycyclic aromatic hydrocarbons using subcritical water extraction coupled with membrane microextraction.

A green analytical methodology for the determination of 16 priority polycyclic aromatic hydrocarbons (PAHs) and 8 related compounds in air particulate matter was developed and validated. The method was based on pressurized hot water extraction (PHWE) followed by miniaturized membrane-assisted solvent extraction (MASE) and programmed temperature vaporization-gas chromatography-ion trap tandem mass spectrometry detection (PTV-GC-MS/MS). The parameters studied for PHWE were percentage of organic modifier (25% MeOH), temperature (200 °C) and static extraction time (5 min). For MASE, extraction temperature (30 °C), time (90 min) and effect of an organic modifier were also optimized. The matrix effect was evaluated and compensated using deuterated labelled standards as surrogates for the quantitation of the target compounds. The analytical performance of the method was satisfactory: relative recoveries varied between 78 and 118% and repeatability and intermediate precision were <22% for all compounds. The Method Quantitation Limits (MQL) ranged from 0.9 (TPY) to 75.6 pg m-3 (NAP). Satisfactory results for accuracy and traceability were evidenced by the analysis of a reference material (SRM 1649b) and comparison with previously published methods. The greenness score was estimated and compared with other techniques widely used for the analysis of PAHs in particulate matter, having a lower relative environmental impact.