Fluidized-bed extraction of polycyclic aromatic hydrocarbons from contaminated soil samples

Chromatographia (Impact Factor: 1.44). 01/2002; 55(7):467-473. DOI: 10.1007/BF02492279

ABSTRACT Due to the carcinogenity and ubiquity of polycyclic aromatic hydrocarbons in the environment they are of ongoing interest
to analytical chemistry. In this study, a comparison of the classic Soxhlet extraction and, fluidized-bed extraction, has
been conducted. The extraction of polycyclic aromatic hydrocarbons by this technique has been optimized considering as experimental
variables the variation of the number of extraction cycles and the holding time after reaching the heating temperature by
means of a surface response design. The significance of the operational parameters of the fluidized-bed extraction on the
performance characteristics has been investigated. For the determination of the analytes a selective clean-up of the extracts
followed by a fast gas chromatography method with mass spectrometric detection was used, resulting in low limits of detection
(0.2 pg μL−1). The accuracy of the complete analytical method was established by extraction and analysis of reference materials.

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    ABSTRACT: An analytical method has been developed for the quantification of two herbicides (ethidimuron and methabenzthiazuron) and their two main soil derivatives. This method involves fluidized-bed extraction (FBE) prior to cleanup and analysis by reverse-phase liquid chromatography with UV detection at 282 nm. FBE conditions were established to provide efficient extraction without degradation of the four analytes. (14)C-labeled compounds were used for the optimization of extraction and purification steps and for the determination of related efficiencies. Extraction was optimal using a fexIKA extractor operating at 110 degrees C for three cycles (total time = 95 min) with 75 g of soil and 150 mL of a 60:40 v/v acetone/water mixture. Extracts were further purified on a 500 mg silica SPE cartridge. Separation was performed on a C18 Purosphere column (250 mm x 4 mm i.d.), at 0.8 mL min(-1) and 30 degrees C with an elution gradient made up of phosphoric acid aqueous solution (pH 2.2) and acetonitrile. Calibration curves were found to be linear in the 0.5-50 mg L(-1) concentration range. Besides freshly spiked soil samples, method validation included the analysis of samples with aged residues. Recovery values, determined from spiked samples, were close to 100%. Limits of detection ranged between 2 and 3 microg kg(-1) of dry soil and limits of quantification between 8 and 10 microg kg(-1) of dry soil. An attempt to improve these performances by using fluorescence detection following postcolumn derivatization by orthophthalaldehyde-mercaptoethanol reagent was unsuccessful.
    Journal of Agricultural and Food Chemistry 11/2006; 54(20):7450-9. · 3.11 Impact Factor
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    ABSTRACT: This paper aims to provide a review of the analytical extraction techniques for polycyclic aromatic hydrocarbons (PAHs) in soils. The extraction technologies described here include Soxhlet extraction, ultrasonic and mechanical agitation, accelerated solvent extraction, supercritical and subcritical fluid extraction, microwave-assisted extraction, solid phase extraction and microextraction, thermal desorption and flash pyrolysis, as well as fluidised-bed extraction. The influencing factors in the extraction of PAHs from soil such as temperature, type of solvent, soil moisture, and other soil characteristics are also discussed. The paper concludes with a review of the models used to describe the kinetics of PAH desorption from soils during solvent extraction.
    International Journal of Analytical Chemistry 01/2010; 2010:398381.