Analytical and Bioanalytical Chemistry

, Volume 387, Issue 7, pp 2569–2583 | Cite as

New strategies to screen for endocrine-disrupting chemicals in the Portuguese marine environment utilizing large volume injection–capillary gas chromatography–mass spectrometry combined with retention time locking libraries (LVI–GC–MS–RTL)

  • C. Almeida
  • P. Serôdio
  • M. H. Florêncio
  • J. M. F. Nogueira
Original Paper


A new analytical strategy to screen for endocrine-disrupting chemicals (EDCs) in environmental matrices is presented. The strategy uses solid-phase extraction followed by large volume injection and capillary gas chromatography coupled to mass spectrometry combined with retention time locking libraries (SPE–LVI–GC–MS–RTL). Characterization of the proposed methodology (SPE–LVI–GC–MS) for selected classes of EDCs enabled high reproducibility and robustness at the ultratrace level. The RTL databases used allowed hundreds of non-target semivolatiles (i.e., pesticides, polycyclic aromatic hydrocarbons, polychlorinated biphenyls and other classes of suspected EDCs from a great number of unknown environmental matrices) to be simultaneously screened for in an easy, fast and remarkable manner. The application of the proposed methodology to real environmental samples demonstrated its remarkable selectivity and sensitivity at the ultratrace level. Screening assessments performed on water and sediment matrices from eight Portuguese estuaries and coastal waters identified EDC “hotspots.” These EDCs mainly come from agricultural and a wide variety of industrial sources, and include pesticides and pesticide metabolites, phenolic derivatives and polycyclic aromatic hydrocarbons, which are included in the lists of priority substances published by international environmental agencies. The estuaries that contained relatively high levels of pesticides were Guadiana, Sado and Mondego, while Minho, Douro and Formosa showed enhanced levels of phenolic derivatives. Dibutyltin and tributyltin, selected as target compounds to be monitored by SPE–LVI–GC–MS in the selected ion monitoring mode, were shown to be widespread contaminants at trace levels in almost all of the sediment matrices assessed. The reliability of the proposed methodology undoubtedly makes it a valuable tool that could replace other analytical strategies currently used to screen for EDCs present in the environment at ultratrace levels.


SPE–LVI–GC–MS RTL databases Endocrine-disrupting chemicals Pesticides and metabolites Phenolic derivatives PAHs Organotins Environmental matrices Portuguese estuaries 



This research was supported by the Fundação para a Ciência e a Tecnologia (PDCTM/C/MAR/15283/1999). We thank Henrique Cabral and his group from Oceanography Institute (FCUL) for sampling in the Douro and Tagus estuaries; José C. Antunes and his group from Marine Investigation Institute (CIIMAR) for sampling in the Minho estuary; Miguel A. Pardal from University of Coimbra (FCTUC) for sampling in the Mondego estuary; Carla Lopes from University of Aveiro for sampling in the Aveiro estuary and Constança Bexiga, Alice Newton and Adelino Canário from the University of Algarve for sampling in the Sado, Guadiana and Formosa estuaries.


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Copyright information

© Springer-Verlag 2007

Authors and Affiliations

  • C. Almeida
    • 1
  • P. Serôdio
    • 1
  • M. H. Florêncio
    • 1
    • 2
  • J. M. F. Nogueira
    • 1
    • 3
  1. 1.Chemistry and Biochemistry DepartmentUniversity of LisbonLisbonPortugal
  2. 2.Center of Chemistry and BiochemistryUniversity of LisbonLisbonPortugal
  3. 3.Center for Molecular Sciences and MaterialsUniversity of LisbonLisbonPortugal

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