PMID- 24679410
OWN - NLM
STAT- MEDLINE
DCOM- 20140816
LR  - 20221207
IS  - 1873-3778 (Electronic)
IS  - 0021-9673 (Linking)
VI  - 1340
DP  - 2014 May 2
TI  - In-port derivatization coupled to different extraction techniques for the 
      determination of alkylphenols in environmental water samples.
PG  - 1-7
LID - S0021-9673(14)00390-2 [pii]
LID - 10.1016/j.chroma.2014.03.013 [doi]
AB  - Large volume injection (LVI)-in port silylation coupled to gas 
      chromatography-mass spectrometry (GC-MS) for the determination of alkylphenols 
      (APs) in water samples applying four different extraction approaches was 
      evaluated. Among the variables studied for in-port derivatization, vent time, 
      cryo-focusing temperature and the ratio solvent 
      volume/N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) volume were optimized 
      using an experimental design approach. Regarding the extraction techniques, 
      different approaches previously optimized in the research group were tested. On 
      the one hand different polymeric materials were tested: silicon rod (SR), 
      polyethersulfone (PES) and polydimethylsiloxane (PDMS), the latter in the 
      stir-bar sorptive extraction format (SBSE-PDMS). PES was chosen among the 
      polymeric materials due to the higher recoveries (compared with SR) and lower 
      price (compared to PDMS in the stir-bar sorptive extraction, SBSE-PDMS). Both 
      MASE and PES protocols were selected at this point for further method validation 
      and application to real samples. Finally, the developed methods were validated 
      and applied to the determination of target analytes in various aqueous 
      environmental matrices, including estuarine water and wastewater. Acceptable 
      repeatability in the case of MASE (5-17%) and PES (7-21%) procedures and method 
      detection limits (MDLs, 5-123 and 28-328 ng L(-1) for PES and MASE, respectively) 
      were obtained for most analytes. In terms of apparent recoveries in the presence 
      of matrix, estuarine and effluent samples showed no significant matrix effect 
      (apparent recoveries in the 73-121% for PES and 74-128% for MASE), while a 
      stronger matrix effect was observed for influent wastewater samples (98-132% for 
      PES and 65-156% for MASE). Both MASE and PES extractions combined with 
      LVI-in-port derivatization-GC-MS were applied to the determination of APs in the 
      estuary of Bilbao (Gulf of Biscay, Spain).
CI  - Copyright (c) 2014 Elsevier B.V. All rights reserved.
FAU - Cavalheiro, J
AU  - Cavalheiro J
AD  - Department of Analytical Chemistry, Faculty of Science and Technology, University 
      of the Basque Country, P. K. 644, 48080, Bilbao, Spain; Laboratoire de Chimie 
      Analytique Bio-inorganique et Environnement, Institut Pluridisciplinaire de 
      Recherche sur l'Environnement et les Materiaux, CNRS UMR 5254, Universite de Pau 
      et des Pays de l'Adour, Helioparc Pau Pyrenees, 2, av. P. Angot, 64053, Pau cedex 
      9, France.
FAU - Monperrus, M
AU  - Monperrus M
AD  - Laboratoire de Chimie Analytique Bio-inorganique et Environnement, Institut 
      Pluridisciplinaire de Recherche sur l'Environnement et les Materiaux, CNRS UMR 
      5254, Universite de Pau et des Pays de l'Adour, Helioparc Pau Pyrenees, 2, av. P. 
      Angot, 64053, Pau cedex 9, France.
FAU - Amouroux, D
AU  - Amouroux D
AD  - Laboratoire de Chimie Analytique Bio-inorganique et Environnement, Institut 
      Pluridisciplinaire de Recherche sur l'Environnement et les Materiaux, CNRS UMR 
      5254, Universite de Pau et des Pays de l'Adour, Helioparc Pau Pyrenees, 2, av. P. 
      Angot, 64053, Pau cedex 9, France.
FAU - Preud'Homme, H
AU  - Preud'Homme H
AD  - Laboratoire de Chimie Analytique Bio-inorganique et Environnement, Institut 
      Pluridisciplinaire de Recherche sur l'Environnement et les Materiaux, CNRS UMR 
      5254, Universite de Pau et des Pays de l'Adour, Helioparc Pau Pyrenees, 2, av. P. 
      Angot, 64053, Pau cedex 9, France.
FAU - Prieto, A
AU  - Prieto A
AD  - Department of Analytical Chemistry, Faculty of Science and Technology, University 
      of the Basque Country, P. K. 644, 48080, Bilbao, Spain.
FAU - Zuloaga, O
AU  - Zuloaga O
AD  - Department of Analytical Chemistry, Faculty of Science and Technology, University 
      of the Basque Country, P. K. 644, 48080, Bilbao, Spain. Electronic address: 
      olatz.zuloaga@ehu.es.
LA  - eng
PT  - Evaluation Study
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
DEP - 20140311
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Acetamides)
RN  - 0 (N,O-bis(trimethylsilyl)trifluoroacetamide)
RN  - 0 (Phenols)
RN  - 0 (Trimethylsilyl Compounds)
RN  - 0 (Waste Water)
RN  - 0 (Water Pollutants, Chemical)
SB  - IM
MH  - Acetamides
MH  - Gas Chromatography-Mass Spectrometry/*methods
MH  - Phenols/*analysis/isolation & purification
MH  - Solid Phase Microextraction
MH  - Temperature
MH  - Trimethylsilyl Compounds
MH  - Wastewater/chemistry
MH  - Water Pollutants, Chemical/*analysis/isolation & purification
OTO - NOTNLM
OT  - Alkylphenols
OT  - Different extraction techniques
OT  - In-port derivatization
OT  - Large volume injection
OT  - Water samples
EDAT- 2014/04/01 06:00
MHDA- 2014/08/17 06:00
CRDT- 2014/04/01 06:00
PHST- 2013/12/24 00:00 [received]
PHST- 2014/03/02 00:00 [revised]
PHST- 2014/03/04 00:00 [accepted]
PHST- 2014/04/01 06:00 [entrez]
PHST- 2014/04/01 06:00 [pubmed]
PHST- 2014/08/17 06:00 [medline]
AID - S0021-9673(14)00390-2 [pii]
AID - 10.1016/j.chroma.2014.03.013 [doi]
PST - ppublish
SO  - J Chromatogr A. 2014 May 2;1340:1-7. doi: 10.1016/j.chroma.2014.03.013. Epub 2014 
      Mar 11.