RT Journal Article
T1 Solid-phase microextraction with simultaneous oxidative sample treatment for the sensitive determination of tetra- to hexa-brominated diphenyl ethers in sediments
A1 Montes Goyanes, Rosa
A1 Rodríguez Pereiro, Isaac
A1 Cela Torrijos, Rafael
K1 Polybrominated diphenyl ethers
K1 Solid-phase microextraction
K1 Sediments
K1 Oxidative sample treatment
K1 Gas chromatography
AB Solid-phase microextraction (SPME) is an effective technique for the extraction of polybrominated diphenyl ethers (PBDEs) from environmental water samples. Although it has been also applied to sediments, the organic content of this matrix causes an exponential decrease in the yield of the extraction. This work presents an improved SPME procedure for the sensitive determination of six PBDEs (tetra- to hexa-brominated congeners) in sediments containing up to 6% of total organic carbon (TOC). Samples (0.25–0.5g) were accurately weighed in 22mL glass vessels, mixed with a given amount of potassium permanganate, 0.5mL of sulphuric acid and 5mL of water. Extractions were performed at 100°C, for 40min, using a polyacrylate (PA) coated fibre in the headspace (HS) mode. Potassium permanganate showed a dramatic, positive effect on the yield of the extraction. Its optimum amount was related to the TOC of the sediment, with overall highest responses attained for 40mg of oxidant per mg of organic carbon in the SPME vessel. Under final working conditions, the combination of SPME with gas chromatography coupled to tandem mass spectrometry (GC–MS/MS) provided relative standard deviations (RSDs) below 14%, relative recoveries from 76 to 111% and limits of quantification (LOQs) lower than 0.15ngg−1 for all the investigated PBDEs in spiked river and marine sediments with different TOC. The performance of the method was also evaluated satisfactorily with a medium complexity (TOC 6.7%), real-life polluted sediment, previously analyzed in inter-laboratory comparison exercises.
PB Elsevier
YR 2009
FD 2009-11-17
LK http://hdl.handle.net/10347/31966
UL http://hdl.handle.net/10347/31966
LA eng
NO Montes, R., Rodríguez, I., Cela, R. Solid-phase microextraction with simultaneous oxidative sample treatment for the sensitive determination of tetra- to hexa-brominated diphenyl ethers in sediments, Journal of Chromatography A, Volume 1217, Issue 1, 2010, Pages 14-21
NO This is the postprint (accepted manuscript) version of the article published in Journal of Chromatography A  https://doi.org/10.1016/j.chroma.2009.11.029  This manuscript version is made available under de CC-BY-NC-ND 4.0 license
NO This study has been supported by the Spanish Government and E.U. FEDER funds (project CTQ2009-08377). R. M. thanks a FPU contract to the Spanish Ministry of Science and Innovation.
DS Minerva
RD 24 abr 2026