Fractionation of chlorinated and brominated persistent organic pollutants in several food samples by pyrenyl-silica liquid chromatography prior to GC-MS determination

Authors
Gómara, Belén; García Ruiz, CarmenUniversity of Alcalá Author; González, María José; Marina Alegre, María LuisaUniversity of Alcalá Author
Identifiers
Permanent link (URI): http://hdl.handle.net/10017/1325
DOI: 10.1016/j.aca.2006.02.053
ISSN: 0003-2670
Publisher
Elsevier
Date
2006
Affiliation
Universidad de Alcalá. Departamento de Química Analítica e Ingeniería Química
Funders
The authors thank the Comunidad Autonoma de Madrid (Spain) for project S-0505/AGR/0312. B. Gomara wishes to thank the University of Alcala and CSIC for her grants and C. Zuniga for her kind help. C. García-Ruiz thanks the Ministry of Science and Technology for the Ramon y Cajal program (RYC-2003-001)
Bibliographic citation
Analytica Chimica Acta, 2006, v. 565, p. 208-213
Keywords
Brominated and chlorinated POPs
Fractionation
PYE
HPLC
Project
S-0505-AGR-0312 (Comunidad de Madrid)
info:eu-repo/grantAgreement/MEC//RYC-2003-001/ES/RYC-2003-001/
Document type
info:eu-repo/semantics/article
Version
info:eu-repo/semantics/publishedVersion
Publisher's version
http://dx.doi.org/10.1016/j.aca.2006.02.053
Rights
(c) Elsevier, 2006
Access rights
info:eu-repo/semantics/openAccess
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Abstract
A high-performance liquid chromatography (HPLC) method using a column of 2-(1-pyrenyl) ethyldimethylsilylated silica was developed in this work in order to achieve satisfactory and reproducible fractionation of polychlorinated biphenyls (PCBs) from brominated flame retardants (BFRs) (polybrominated diphenylethers, PBDEs; and polybrominated biphenyls, PBBs). After the study of different chromatographic parameters (mobile phase composition and separation temperature were the most important) an isocratic elution with isooctane:toluene (98:2, v/v) at a flow-rate of 1 mL/min, a temperature of 45 °C, and UV-detection at 225 nm was selected for fractionation of PCBs (time region, 4.0–5.8 min) from PBDEs (5.8–9.0 min) and from PBBs (5.8–11.0 min). The applicability of this method to food samples was demonstrated by fractionating PCBs from PBDEs in three food samples (cheese, milk, and fish). Interferences from PCBs (present in real samples at much higher concentrations than PBDEs) were removed in this way. In addition, by analysing these samples by gas chromatography–mass spectrometry (GC–MS) with and without previous fractionation we were able to observe an improvement in detection sensitivity for PBDEs after HPLC fractionation.
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