Rapid method for the determination of polycyclic aromatic hydrocarbons in agricultural soils by sonication-assisted extraction in small columns
A rapid method has been developed for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in soil based on their sonication-assisted extraction in small columns (SAESC) with a low volume of ethyl acetate and subsequent quantitation and identification by GC with electron impact mass spectrometric detection in the SIM mode (GC-MS-SIM). Spiked blank soil extracts were used as standards to counter-act the matrix effect observed in the chromatographic determination. PAHs were confirmed at trace level by their retention times, their qualifier and target ions, and their qualifier/target abundance ratios. Recovery studies were performed at 0.5, 1.0, 5.0, and 10 μg/kg fortification levels for each PAH, and the recoveries obtained ranged from 91.2 to 99.8% with RSDs between 0.4 and 9.3%. The detection limits of the method ranged from 0.03 to 0.3 μg/kg for the different PAHs studied. The developed method is linear over the range assayed, 1-100 μg/L with determination coefficients higher than 0.996. PAH levels were determined using this method in soil samples taken from different agricultural areas of Spain. In general, PAH concentrations were low and the most frequently occurring PAHs were naphthalene, pyrene, phenanthrene, and fluoranthene. © 2006 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.
| Main Authors: | , , |
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| Format: | artículo biblioteca |
| Language: | English |
| Published: |
Wiley
2006
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| Subjects: | C-MS, Polycyclic aromatic hydrocarbons, Sonication-assisted extraction in small collumns, Soil, Sonication, |
| Online Access: | http://hdl.handle.net/20.500.12792/5465 http://hdl.handle.net/10261/292282 |
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| Summary: | A rapid method has been developed for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in soil based on their sonication-assisted extraction in small columns (SAESC) with a low volume of ethyl acetate and subsequent quantitation and identification by GC with electron impact mass spectrometric detection in the SIM mode (GC-MS-SIM). Spiked blank soil extracts were used as standards to counter-act the matrix effect observed in the chromatographic determination. PAHs were confirmed at trace level by their retention times, their qualifier and target ions, and their qualifier/target abundance ratios. Recovery studies were performed at 0.5, 1.0, 5.0, and 10 μg/kg fortification levels for each PAH, and the recoveries obtained ranged from 91.2 to 99.8% with RSDs between 0.4 and 9.3%. The detection limits of the method ranged from 0.03 to 0.3 μg/kg for the different PAHs studied. The developed method is linear over the range assayed, 1-100 μg/L with determination coefficients higher than 0.996. PAH levels were determined using this method in soil samples taken from different agricultural areas of Spain. In general, PAH concentrations were low and the most frequently occurring PAHs were naphthalene, pyrene, phenanthrene, and fluoranthene. © 2006 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim. |
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