PMID- 18761165
OWN - NLM
STAT- MEDLINE
DCOM- 20081030
LR  - 20080901
IS  - 1873-3573 (Electronic)
IS  - 0039-9140 (Linking)
VI  - 76
IP  - 5
DP  - 2008 Sep 15
TI  - An expeditious method for the determination of organochlorine pesticides residues 
      in estuarine sediments using microwave assisted pre-extraction and automated 
      headspace solid-phase microextraction coupled to gas chromatography-mass 
      spectrometry.
PG  - 1124-9
LID - 10.1016/j.talanta.2008.05.035 [doi]
AB  - Determination of organochlorine pesticides (OCPs) in sediments implicates 
      extraction of these compounds from the matrix, which is difficult owing to strong 
      interaction among OCPs and different constituents of the sediments, particularly 
      organic content. The method here described is a combination of microwave assisted 
      extraction (MAE), headspace solid-phase microextraction (HS-SPME) and gas 
      chromatography-mass spectrometry (GC-MS), acting in selected-ion storage mode, or 
      GC-electron capture detector (ECD, for routine analysis). Methanol was used as 
      extracting solvent and aliquots of the MAE extracts (after inclusion of a step 
      for sulfur elimination when required) were used to prepare aqueous solutions for 
      HS-SPME. A complete automation of the SPME procedure increases the sample 
      throughput, including standard addition for calibration purpose. The procedure 
      has the advantage of exclude additional clean-up steps and pre-concentration 
      before SPME. Application to reference sediments of different characteristics 
      revealed absence of significant interferences from the matrix for alpha-lindane, 
      gamma-lindane, aldrin, dieldrin, endrin, 4,4'-DDT, 4,4'-DDD, 4,4'-DDE, 
      heptachlor, heptachlor epoxide and good sensitivity. Detection limits ranged from 
      0.005 to 0.11 ng of OCP per gram of dried sediment using GC-MS and from 0.01 to 
      0.26 ngg(-1) using GC-ECD. The linear response ranges embraced 5-6 orders of 
      magnitude (up to 1000 ngg(-1)) in GC-MS, being narrower for GC-ECD. The method 
      was successfully applied to sandy and muddy sediments from Portuguese rivers 
      estuaries, enabling quantification of seven OCPs. The method resulted effective, 
      relatively simple and fast, being suitable for routine monitoring of residues of 
      OCPs from sediments of different grain size and organic matter content, which 
      influence concentration, mobility and availability of contaminants.
FAU - Carvalho, Pedro N
AU  - Carvalho PN
AD  - CIMAR/CIIMAR - Centro Interdisciplinar de Investigacao Marinha e Ambiental and 
      Faculdade de Ciencias, Universidade do Porto, R. Campo Alegre 687, Porto 
      4169-007, Portugal.
FAU - Rodrigues, Pedro Nuno R
AU  - Rodrigues PN
FAU - Alves, Filipe
AU  - Alves F
FAU - Evangelista, Rafael
AU  - Evangelista R
FAU - Basto, Maria Clara P
AU  - Basto MC
FAU - Vasconcelos, M Teresa S D
AU  - Vasconcelos MT
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
DEP - 20080707
PL  - Netherlands
TA  - Talanta
JT  - Talanta
JID - 2984816R
RN  - 0 (Hydrocarbons, Chlorinated)
RN  - 0 (Pesticide Residues)
SB  - IM
MH  - Automation
MH  - Calibration
MH  - Gas Chromatography-Mass Spectrometry
MH  - Geologic Sediments/*chemistry
MH  - Hydrocarbons, Chlorinated/*analysis/chemistry
MH  - *Microwaves
MH  - Particle Size
MH  - Pesticide Residues/*analysis/chemistry
MH  - Reproducibility of Results
MH  - Rivers/chemistry
MH  - Solid Phase Microextraction/*methods
MH  - Time Factors
EDAT- 2008/09/02 09:00
MHDA- 2008/10/31 09:00
CRDT- 2008/09/02 09:00
PHST- 2008/01/17 00:00 [received]
PHST- 2008/05/09 00:00 [revised]
PHST- 2008/05/14 00:00 [accepted]
PHST- 2008/09/02 09:00 [pubmed]
PHST- 2008/10/31 09:00 [medline]
PHST- 2008/09/02 09:00 [entrez]
AID - S0039-9140(08)00397-4 [pii]
AID - 10.1016/j.talanta.2008.05.035 [doi]
PST - ppublish
SO  - Talanta. 2008 Sep 15;76(5):1124-9. doi: 10.1016/j.talanta.2008.05.035. Epub 2008 
      Jul 7.