PMID- 16714025
OWN - NLM
STAT- MEDLINE
DCOM- 20060920
LR  - 20131121
IS  - 0021-9673 (Print)
IS  - 0021-9673 (Linking)
VI  - 1124
IP  - 1-2
DP  - 2006 Aug 18
TI  - Rapid screening of polychlorinated biphenyls in sediments using non-equilibrium 
      solid-phase microextraction and fast gas chromatography with electron-capture 
      detection.
PG  - 43-50
AB  - A rapid method for the screening of polychlorinated biphenyls (PCBs) in sediment 
      samples is described. Analytes are concentrated on a poly(dimethylsiloxane) 
      (PDMS) solid-phase microextraction (SPME) fibre, separated using a narrow-bore 
      gas chromatography column (10 m x 0.1mm I.D.) and determined with a 
      micro-electron-capture detector (micro-ECD). The narrow-bore column showed a 
      similar separation efficiency to a conventional capillary one (30 m x 0.32 mm 
      I.D.) and allowed a 3 times reduction in the analysis time. Moreover, thermal 
      desorption of SPME fibres in the narrow-bore column did not produce any 
      degradation in the quality of separations when compared to the split injection 
      mode. The use of an oxidative sample treatment was mandatory to remove sulphur 
      interferences in the chromatograms and increase the yield of PCBs during SPME for 
      short sampling times. Under optimised conditions, a fraction of sediment (0.1-0.5 
      g) was mixed with 5 ml of a 0.2M potassium permanganate solution and 0.5 ml of 
      sulphuric acid 6M in a 22 ml closed vessel. Sample treatment and headspace SPME 
      of PCBs were performed simultaneously for 10 min at 100 degrees C. Globally, the 
      whole analytical procedure takes about 20 min and presents quantification limits 
      between 0.5 and 1.3 ng/g. Accuracy was evaluated by analysing a reference 
      sediment sample with certified concentrations of several PCBs.
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 - Ramil, M
AU  - Ramil M
FAU - Rodriguez, I
AU  - Rodriguez I
FAU - Rubi, E
AU  - Rubi E
FAU - Cela, R
AU  - Cela R
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
DEP - 20060519
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - DFC2HB4I0K (Polychlorinated Biphenyls)
SB  - IM
MH  - Chromatography, Gas/*methods
MH  - Geologic Sediments/*chemistry
MH  - Kinetics
MH  - Polychlorinated Biphenyls/*analysis
EDAT- 2006/05/23 09:00
MHDA- 2006/09/21 09:00
CRDT- 2006/05/23 09:00
PHST- 2006/02/03 00:00 [received]
PHST- 2006/04/19 00:00 [revised]
PHST- 2006/04/21 00:00 [accepted]
PHST- 2006/05/23 09:00 [pubmed]
PHST- 2006/09/21 09:00 [medline]
PHST- 2006/05/23 09:00 [entrez]
AID - S0021-9673(06)00865-X [pii]
AID - 10.1016/j.chroma.2006.04.047 [doi]
PST - ppublish
SO  - J Chromatogr A. 2006 Aug 18;1124(1-2):43-50. doi: 10.1016/j.chroma.2006.04.047. 
      Epub 2006 May 19.