Static pressurised liquid extraction of nitrated polycyclic aromatic hydrocarbons from soils with on-line filtration-preconcentration prior to gas chromatography-mass spectrometry detection.
Nitrated polycyclic aromatic hydrocarbons have been extracted from both spiked and natural contaminated soils by using static pressurised liquid extraction. The variables governing the extraction (namely, pressure, extraction time, temperature and number of static extraction cycles) have been optimised using the experimental design methodology. A laboratory-made pressurised liquid extractor has been used allowing its coupling to a filtration-preconcentration system through a flow injection interface, thus providing a partially automated approach. Gas chromatography with MS-MS ion preparation mode has been used for individual separation-identification/quantification providing both high selectivity (no interferences were observed) and sensitivity (detection limits of low pg). The comparison of the proposed approach with the reference EPA Method 3540 has shown that both methods provide similar efficiencies but with dramatic saving of time by the former (30 min vs. 24 h). The use of water as leaching agent avoids the use of organic solvents, thus providing an environmentally friendly method.
Luque-García
J L
JL
Department of Analytical Chemistry, Marie Curie Building (Annex), Campus of Rabanales, University of Córdoba, E-14071 Córdoba, Spain. q52lugaj@uco.es
Luque de Castro
M D
MD
D005374:Filtration / Q000379:methods; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D011084:Polycyclic Aromatic Hydrocarbons / Q000302:isolation & purification*; D012987:Soil / Q000032:analysis*; D012989:Soil Pollutants / Q000302:isolation & purification*
D011084:Polycyclic Aromatic Hydrocarbons; D012987:Soil; D012989:Soil Pollutants