Miniaturised pressurised liquid extraction of polycyclic aromatic hydrocarbons from soil and sediment with subsequent large-volume injection-gas chromatography

J Chromatogr A. 2000 Sep 8;891(2):275-86. doi: 10.1016/s0021-9673(00)00652-x.

Abstract

Analyte extraction is the main limitation when developing at-line, or on-line, procedures for the preparation of (semi)solid environmental samples. Pressurised liquid extraction (PLE) is an analyte- and matrix-independent technique which provides cleaner extracts than the time-consuming classical procedures. In the study, the practicality of miniaturised PLE performed in a stainless-steel cell, and combined with subsequent large-volume injection (LVI)-GC-MS was studied. As an example, the new system was applied to the determination of polycyclic aromatic hydrocarbons (PAHs) in soils and a sediment. Variables affecting the PLE efficiency, such as pressure and temperature of the extraction solvent and total solvent volume, were studied. Toluene was selected as extraction solvent and a total solvent volume of 100 microl was used for the 10 min static-dynamic PLE of 50-mg samples. Additional clean-up or filtration of the sample extracts was not required. Detection limits using LVI-GC-MS were below 9 ng/g soil for the 13 PAHs more volatile than indeno[1,2,3-cd]pyrene in real soil samples and the repeatability of the complete PLE plus LVI-GC-MS method for the analysis of the endogenous PAH was better than 15%. Comparison of PLE and Soxhlet or liquid-partitioning extraction results for the analysis of non-spiked samples showed that the efficiency of PLE is the same or better than for the other two extraction methods assayed.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Gas Chromatography-Mass Spectrometry / methods*
  • Hydrocarbons, Aromatic / analysis*
  • Hydrocarbons, Aromatic / isolation & purification
  • Miniaturization
  • Reproducibility of Results
  • Soil Pollutants / analysis*
  • Soil Pollutants / isolation & purification

Substances

  • Hydrocarbons, Aromatic
  • Soil Pollutants