An ultrasound-assisted pressure-regulated solid-phase microextraction setup for fast and sensitive analysis of volatile pollutants in contaminated soil.

Release of analytes from their native matrix and diffusion into the gas phase is the rate-limiting step for the sampling of volatiles in complex solid samples. This limitation is more serious in the solvent-less and solvent-free microextraction sampling strategies. In this research, a three-stage reinforced sampling strategy including high-pressure/sonication/low-pressure was introduced for fast and efficient release of analytes in soil samples. For this purpose, a novel ultrasound-assisted pressure-regulated solid-phase microextraction (UA-PR-SPME) device was developed. It was coupled with gas chromatography-flame ionization detection (GC-FID) and carried out for the determination of benzene, toluene, ethylbenzene, and xylenes (BTEX, as the model analytes) in complex solid samples. Graphene oxide/3-aminopropyltriethoxysilane (GO-APTES) nanocomposite was synthesized and used as the SPME fiber coating. Under optimal conditions, the limits of detection (LODs) were obtained 0.1-0.4 ng/g. The calibration curves were linear over the range of 2.4-5000 ng/g. Relative standard deviations (RSDs%) were calculated 5.1-7.0% (n = 6). The developed technique was employed for the analysis of BTEX in contaminated soil samples.