Miniaturised pressurised liquid extraction of chloroanilines from soil with subsequent analysis by large-volume injection–gas chromatography–mass spectrometry

A number of chloroanilines were extracted from soil by means of miniaturised pressurised liquid extraction (PLE). The extraction procedure was optimised for both large-volume on-column (LV-OC) and programmed-temperature vaporisation (PTV) injections combined with GC–MS. Hexane was the only extraction solvent suited for LV-OC and hexane/acetone gave the best results when using a PTV. Overall, the hexane/acetone-plus-PTV procedure shows better results than the hexane-plus-LV-OC method in terms of analyte recovery (36–109% versus 5–87%), repeatability (8–13% versus 4–31%) and detection limits. Both approaches allow detection of the chloroanilines in complex soil samples down to the 5–50 ng/g range. However, the PTV-based procedure is superior as regards robustness: over one hundred samples can be analysed without any maintenance being required.