PMID- 19945111
OWN - NLM
STAT- MEDLINE
DCOM- 20100223
LR  - 20191210
IS  - 1873-3778 (Electronic)
IS  - 0021-9673 (Linking)
VI  - 1217
IP  - 1
DP  - 2010 Jan 1
TI  - Solid-phase microextraction with simultaneous oxidative sample treatment for the 
      sensitive determination of tetra- to hexa-brominated diphenyl ethers in 
      sediments.
PG  - 14-21
LID - 10.1016/j.chroma.2009.11.029 [doi]
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 degrees 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.
CI  - Copyright 2009 Elsevier B.V. All rights reserved.
FAU - Montes, R
AU  - Montes R
AD  - Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de 
      Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, 
      Santiago de Compostela 15782, Spain.
FAU - Rodriguez, I
AU  - Rodriguez I
FAU - Cela, R
AU  - Cela R
LA  - eng
PT  - Evaluation Study
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
DEP - 20091117
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Environmental Pollutants)
RN  - 0 (Halogenated Diphenyl Ethers)
SB  - IM
MH  - Environmental Pollutants/*chemistry
MH  - Gas Chromatography-Mass Spectrometry
MH  - Geologic Sediments/*chemistry
MH  - Halogenated Diphenyl Ethers/*chemistry
MH  - Oxidation-Reduction
MH  - Solid Phase Microextraction/*methods
EDAT- 2009/12/01 06:00
MHDA- 2010/02/24 06:00
CRDT- 2009/12/01 06:00
PHST- 2009/09/11 00:00 [received]
PHST- 2009/11/09 00:00 [revised]
PHST- 2009/11/10 00:00 [accepted]
PHST- 2009/12/01 06:00 [entrez]
PHST- 2009/12/01 06:00 [pubmed]
PHST- 2010/02/24 06:00 [medline]
AID - S0021-9673(09)01690-2 [pii]
AID - 10.1016/j.chroma.2009.11.029 [doi]
PST - ppublish
SO  - J Chromatogr A. 2010 Jan 1;1217(1):14-21. doi: 10.1016/j.chroma.2009.11.029. Epub 
      2009 Nov 17.