Published:Journal of Chromatographic Science,
ISSN 0021-9665Volume
38, Number 2, February 2000, pp. 55–60
Determination
of Polycyclic Aromatic Hydrocarbons in Sediment Using Solid-Phase Microextraction
with Gas ChromatographyÐMass SpectrometryD.
Cam, S. Gagni, L. Meldolesi, and G. Galletti Environmental Research Center Montecatini, Marina
di Ravenna, Italy; Course of Environmental Science, University of Bologna, Italy;
and Dipartment of Chemistry "G. Ciamician", University of Bologna,
Italy
Manual
solid-phase microextraction (SPME) coupled with gas chromatographyÐmass spectrometry
(GC–MS) is applied for the determination of polycyclic aromatic hydrocarbons
(PAHs) from natural matrix through a distilled water medium. Seven of the 16
PAH standards (naphthalene, acenaphthene, fluorene, anthracene, fluoranthene,
pyrene, benzo[a]anthracene) are spiked on a marine
muddy sediment. The samples, containing PAHs in the range of 10–20 ppm,
are then aged at room temperature more than 10 days before analysis. The influence
of the matrix, SPME adsorption time, pH, salt content, and SPME adsorption temperature
are investigated. The reproducibility of the technique is less than 13% (RDS)
for the first 6 considered PAHs and 28% (RDS) for benzo(a)anthracene
with a fiber containing a 100-µm poly dimethylsiloxane coating. Linearity extended
in the range of 5–50 picograms for PAHs direct injection, 5–70 picograms
for PAHs in water, and 1–170 picograms for PAHs in sediment. The detection
limit is estimated less than 1 µg/kg of dry sample for the first 6 considered
PAHs in sediment and 1.5 µg/kg of dry sample for benzo(a)anthracene
using the selected ion monitoring mode in GC–MS. The recoveries of the
considered PAHs are evaluated.
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