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Application of polydimethylsiloxane rod extraction to the determination of sixteen halogenated flame retardants in water samples

An extraction and preconcentration procedure for the determination in water samples of several halogenated flame retardants (FRs), nine brominated diphenyls ethers (BDEs) and seven non-BDE FRs, was developed and validated. The optimised procedure is based on polydimethylsiloxane (PDMS) rods as sorptive extraction material, followed by liquid desorption and gas chromatography coupled to negative chemical ionisation-mass spectrometry (GC-NCI-MS) determination, rendering an efficient and inexpensive method. The final optimised protocol consists of overnight extraction of 100mL of sample solutions containing 40% MeOH and 4% NaCl, followed by a 15-min sonication-assisted desorption with 300μL of ethyl acetate, solvent evaporation and GC-NCI-MS analysis. Under these conditions, extraction efficiencies in the 9 to 70% range were obtained, leading to enrichment factors between 108 and 840, detection limits in the range from 0.4 to 10ngL-1and RSD values in the 2-23% range. After method validation, different real water samples, including river, ria, sea, landfill leachate, influent and effluent wastewater from an urban sewage treatment plant (STP) and effluent wastewater from a textile industry, were analysed. BDE-47, BDE-99, BDE-100 and BDE-197 were detected in wastewater and landfill leachate samples at concentration levels up to 2887ngL-1. Among the non-BDE FRs, bis (2-ethylhexyl)-3,4,5,6-tetrabromo-phthalate (DEHTBP) was detected in surface water samples (sea, river and ria) between 1.3 and 2.2ngL-1 and 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE) in the landfill leachate (64ngL-1)

This work was supported by the Spanish Ministry of Science and Innovation (Ministerio de Ciencia e Innovacion) and FEDER funds, project no. CTQ2009-08377 and CTM2011-28765-C02-02, and Xunta de Galicia, project no.10MDS700006PR. R. Rodil and J.B. Quintana (Ramon y Cajal research program), E. Villaverde-de-Sdaa (FPI grant, ref. BES-2011-047887) and C. Valls-Cantenys (FPI grant, ref. BES-2009-024892) extend their gratitude to the Spanish Ministry of Science and Innovation

© Analytica Chimica Acta, 2013, vol. 770, p. 85-93

Elsevier Masson

Author: Valls Cantenys, Carme
Villaverde-de-Sáa, Eugenia
Rodil, Rosario
Quintana, José Benito
Iglesias Juncà, Mònica
Salvadó Martín, Victòria
Cela, Rafael
Date: 2013 April 3
Abstract: An extraction and preconcentration procedure for the determination in water samples of several halogenated flame retardants (FRs), nine brominated diphenyls ethers (BDEs) and seven non-BDE FRs, was developed and validated. The optimised procedure is based on polydimethylsiloxane (PDMS) rods as sorptive extraction material, followed by liquid desorption and gas chromatography coupled to negative chemical ionisation-mass spectrometry (GC-NCI-MS) determination, rendering an efficient and inexpensive method. The final optimised protocol consists of overnight extraction of 100mL of sample solutions containing 40% MeOH and 4% NaCl, followed by a 15-min sonication-assisted desorption with 300μL of ethyl acetate, solvent evaporation and GC-NCI-MS analysis. Under these conditions, extraction efficiencies in the 9 to 70% range were obtained, leading to enrichment factors between 108 and 840, detection limits in the range from 0.4 to 10ngL-1and RSD values in the 2-23% range. After method validation, different real water samples, including river, ria, sea, landfill leachate, influent and effluent wastewater from an urban sewage treatment plant (STP) and effluent wastewater from a textile industry, were analysed. BDE-47, BDE-99, BDE-100 and BDE-197 were detected in wastewater and landfill leachate samples at concentration levels up to 2887ngL-1. Among the non-BDE FRs, bis (2-ethylhexyl)-3,4,5,6-tetrabromo-phthalate (DEHTBP) was detected in surface water samples (sea, river and ria) between 1.3 and 2.2ngL-1 and 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE) in the landfill leachate (64ngL-1)
This work was supported by the Spanish Ministry of Science and Innovation (Ministerio de Ciencia e Innovacion) and FEDER funds, project no. CTQ2009-08377 and CTM2011-28765-C02-02, and Xunta de Galicia, project no.10MDS700006PR. R. Rodil and J.B. Quintana (Ramon y Cajal research program), E. Villaverde-de-Sdaa (FPI grant, ref. BES-2011-047887) and C. Valls-Cantenys (FPI grant, ref. BES-2009-024892) extend their gratitude to the Spanish Ministry of Science and Innovation
Format: application/pdf
ISSN: 0003-2670
Document access: http://hdl.handle.net/10256/11535
Language: eng
Publisher: Elsevier Masson
Collection: MICINN/PN 2012-2012/CTM2011-28765-C02-02
MICINN/PN 2010-2012/CTQ2009-08377
Reproducció digital del document publicat a: http://dx.doi.org/10.1016/j.aca.2013.01.059
Articles publicats (D-Q)
Is part of: © Analytica Chimica Acta, 2013, vol. 770, p. 85-93
Rights: Tots els drets reservats
Subject: Cromatografia de líquids
Liquid chromatography
Extracció (Química)
Title: Application of polydimethylsiloxane rod extraction to the determination of sixteen halogenated flame retardants in water samples
Type: info:eu-repo/semantics/article
Repository: DUGiDocs

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