PMID- 20685478
OWN - NLM
STAT- MEDLINE
DCOM- 20110104
LR  - 20100805
IS  - 1873-3573 (Electronic)
IS  - 0039-9140 (Linking)
VI  - 82
IP  - 1
DP  - 2010 Jun 30
TI  - Ultrasound-assisted leaching-dispersive solid-phase extraction followed by 
      liquid-liquid microextraction for the determination of polybrominated diphenyl 
      ethers in sediment samples by gas chromatography-tandem mass spectrometry.
PG  - 359-66
LID - 10.1016/j.talanta.2010.04.050 [doi]
AB  - Ultrasound-assisted leaching-dispersive solid-phase extraction followed by 
      dispersive liquid-liquid microextraction (USAL-DSPE-DLLME) technique has been 
      developed as a new analytical approach for extracting, cleaning up and 
      preconcentrating polybrominated diphenyl ethers (PBDEs) from sediment samples 
      prior gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis. In the 
      first place, PBDEs were leached from sediment samples by using acetone. This 
      extract was cleaned-up by DSPE using activated silica gel as sorbent material. 
      After clean-up, PBDEs were preconcentrated by using DLLME technique. Thus, 1 mL 
      acetone extract (disperser solvent) and 60 microL carbon tetrachloride 
      (extraction solvent) were added to 5 mL ultrapure water and a DLLME technique was 
      applied. Several variables that govern the proposed technique were studied and 
      optimized. Under optimum conditions, the method detection limits (MDLs) of PBDEs 
      calculated as three times the signal-to-noise ratio (S/N) were within the range 
      0.02-0.06 ng g(-1). The relative standard deviations (RSDs) for five replicates 
      were <9.8%. The calibration graphs were linear within the concentration range of 
      0.07-1000 ng g(-1) for BDE-47, 0.09-1000 ng g(-1) for BDE-100, 0.10-1000 ng g(-1) 
      for BDE-99 and 0.19-1000 ng g(-1) for BDE-153 and the coefficients of estimation 
      were > or =0.9991. Validation of the methodology was carried out by standard 
      addition method at two concentration levels (0.25 and 1 ng g(-1)) and by 
      comparing with a reference Soxhlet technique. Recovery values were > or =80%, 
      which showed a satisfactory robustness of the analytical methodology for 
      determination of low PBDEs concentration in sediment samples.
CI  - Copyright 2010 Elsevier B.V. All rights reserved.
FAU - Fontana, Ariel R
AU  - Fontana AR
AD  - Grupo de Investigacion y Desarrollo en Quimica Analitica, Av. Ruiz Leal S/N, 
      Parque General San Martin, 5500 Mendoza, Argentina.
FAU - Lana, Nerina B
AU  - Lana NB
FAU - Martinez, Luis D
AU  - Martinez LD
FAU - Altamirano, Jorgelina C
AU  - Altamirano JC
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
DEP - 20100520
PL  - Netherlands
TA  - Talanta
JT  - Talanta
JID - 2984816R
RN  - 0 (Environmental Pollutants)
RN  - 0 (Halogenated Diphenyl Ethers)
RN  - 0 (Solvents)
SB  - IM
MH  - Environmental Pollutants/analysis/isolation & purification
MH  - Gas Chromatography-Mass Spectrometry/*methods
MH  - Geologic Sediments/*chemistry
MH  - Halogenated Diphenyl Ethers/*analysis/*isolation & purification
MH  - Linear Models
MH  - Reproducibility of Results
MH  - Solid Phase Extraction/*methods
MH  - Solvents/chemistry
MH  - Temperature
MH  - Time Factors
MH  - *Ultrasonics
EDAT- 2010/08/06 06:00
MHDA- 2011/01/05 06:00
CRDT- 2010/08/06 06:00
PHST- 2010/03/12 00:00 [received]
PHST- 2010/04/22 00:00 [revised]
PHST- 2010/04/23 00:00 [accepted]
PHST- 2010/08/06 06:00 [entrez]
PHST- 2010/08/06 06:00 [pubmed]
PHST- 2011/01/05 06:00 [medline]
AID - S0039-9140(10)00324-3 [pii]
AID - 10.1016/j.talanta.2010.04.050 [doi]
PST - ppublish
SO  - Talanta. 2010 Jun 30;82(1):359-66. doi: 10.1016/j.talanta.2010.04.050. Epub 2010 
      May 20.