TITLE

Use of experimental design in the optimisation of stir bar sorptive extraction followed by thermal desorption for the determination of brominated flame retardants in water samples

AUTHOR(S)
Prieto, A.; Zuloaga, O.; Usobiaga, A.; Etxebarria, N.; Fernández, L. A.
PUB. DATE
January 2008
SOURCE
Analytical & Bioanalytical Chemistry;Jan2008, Vol. 390 Issue 2, p739
SOURCE TYPE
Academic Journal
DOC. TYPE
Article
ABSTRACT
A method for the determination of polybrominated diphenyl ethers (PBDEs) and polybrominated biphenyls (PBBs) in water samples is proposed. The method involving stir bar sorptive extraction (SBSE) and thermal desorption followed by gas chromatography coupled with mass spectrometry was optimised using statistical design of experiments. In the first place, the influence of different polydimethylsiloxane stir bars was studied. A Plackett–Burman design was chosen to estimate the influence of five factors on the efficiency of the SBSE process: desorption time (5–10 min), desorption temperature (250–300 °C), desorption flow (50–100 mL min−1), cryofocusing temperature (-130 to 40 °C) and vent pressure (0–12.8 psi). Afterwards, two central composite designs were used to find the optimal process settings that were applied to the optimisation of both desorption and extraction efficiency. In the case of the desorption parameters, long desorption times (10 min) and desorption flows lower than 70 mL min-1 yielded the best signals for the majority of compounds. However, different behaviour among the analytes was observed for the vent pressure and we decided to fix it at an intermediate value (7 psi). In the case of extraction parameters, the sample volume and the addition of NaCl did not have a significant effect, while the addition of methanol yielded better extraction responses. Remarkable recovery (82–106%) and repeatability (less than 18%) were attained. Furthermore, excellent regression coefficients ( r 2 = 0.991–0.999) and low detection limits (1.1–6.0 ng L−1) were also achieved for the congeners studied. The proposed method was applied to the analyses of PBDEs and PBBs in waters from the Basque Country, Spain.
ACCESSION #
28110524

 

Related Articles

  • Toxicokinetics of Polybrominated Diphenyl Ether Congeners 47, 99, 100, and 153 in Mice. Staskal, Daniele F.; Hakk, Heldur; Bauer, Daniel; Diliberto, Janet J.; Birnbaum, Linda S. // Toxicological Sciences;Nov2006, Vol. 94 Issue 1, p28 

    The congener profiles of polybrominated diphenyl ethers (PBDEs) in human and wildlife samples are dominated by brominated diphenyl ether (BDE) congeners 47, 99, 100, 153, and 154, all of which are components of the commercial pentaBDE mixtures commonly used in a variety of flammable consumer...

  • Preparation of reference materials for the determination of RoHS-relevant flame retardants in styrenic polymers. Pöhlein, Manfred; Bertran, Raquel Urpi; Wolf, Marion; Van Eldik, Rudi // Analytical & Bioanalytical Chemistry;May2009, Vol. 394 Issue 2, p583 

    Reference materials for the analysis of polybrominated diphenyl ethers, polybrominated biphenyls and other common brominated flame retardants (FR) in styrenic polymers were prepared to suit the demands of actual restriction of the use of certain hazardous substances in electrical and electronic...

  • Salmon Study Raises PBDE Concern. Sissell, Kara // Chemical Week;8/18/2004, Vol. 166 Issue 27, p41 

    Reports on the concerns raised by the findings of a study of brominated flame retardants in salmon from different parts of the world. Necessity of considering whether the primary polybrominated diphenyl ether (PBDE) exposure pathway for humans is through inhalation; Actions taken by the U.S....

  • Polybrominated diphenyl ethers in an advanced wastewater treatment plant. Part 2: Potential effects on a unique aquatic system. Ikonomou, Michael G; Rayne, Sierra // Journal of Environmental Engineering & Science;Sep2005, Vol. 4 Issue 5, p369 

    Concentrations of the mono- through deca-substituted polybrominated diphenyl ether (PBDE) flame retardants were determined in the aqueous effluent from a tertiary-level wastewater treatment plant (WWTP) that uses post-filtration ultraviolet light disinfection. The WWTP is located in a semi-arid...

  • Flame retardants in indoor air -- are they worth it? Barron, Wendy // Air Quality & Climate Change;May2012, Vol. 46 Issue 2, p6 

    The author questions the effectivity of polybrominated diphenyl ethers (PBDEs) as fire retardants in everyday products. Although these substances have been claimed to reduce the number of lives lost from fires, the author says there is little genuine evidence to support this claim. She adds that...

  • Polybrominated diphenyl ethers in an advanced wastewater treatment plant. Part 1: Concentrations, patterns, and influence of treatment processes. Rayne, Sierra; Ikonomou, Micheal G. // Journal of Environmental Engineering & Science;Sep2005, Vol. 4 Issue 5, p353 

    Concentrations and patterns of the mono- through deca-substituted polybrominated diphenyl ether (PBDE) flame retardants were determined in all major unit operations and processes within a tertiary-level wastewater treatment plant (WWTP) having post-filtration ultraviolet light disinfection. The...

  • Body Burdens of Polybrominated Diphenyl Ethers among Urban Anglers. Morland, Kimberly B.; Landrigan, Philip J.; Sjödin, Andreas; Gobeille, Alayne K.; Jones, Richard S.; McGahee, Ernest E.; Needham, Larry L.; Patterson Jr., Donald G. // Environmental Health Perspectives;Dec2005, Vol. 113 Issue 12, p1689 

    Polybrominated diphenyl ethers (PBDEs) have been widely used in the United States and worldwide as flame retardants. Recent PBDE production figures show that worldwide use has increased. To determine whether fish consumption is a source of PBDE exposure for humans, a cross-sectional...

  • Headspace solid-phase microextraction gas chromatography tandem mass spectrometry for the determination of brominated flame retardants in environmental solid samples. Salgado-Petinal, Carmen; Garcia-Chao, Maria; Llompart, Maria; Garcia-Jares, Carmen; Cela, Rafael // Analytical & Bioanalytical Chemistry;Jul2006, Vol. 385 Issue 3, p637 

    A headspace solid-phase microextraction gas chromatography coupled with tandem mass spectrometry (HSSPME-GC-MS-MS) methodology for determination of brominated flame retardants in sediment and soil samples is presented. To the best of our knowledge, this is the first time that SPME has been...

  • Different Levels of Polybrominated Diphenyl Ethers (PBDEs) and Chlorinated Compounds in Breast Milk from Two U.K. Regions. Kalantzi, Olga I.; Martin, Francis L.; Thomas, Gareth O.; Alcock, Ruth E.; Tang, Huiru R.; Drury, Suzanne C.; Carmichael, Paul L.; Nicholson, Jeremy K.; Jones, Kevin C. // Environmental Health Perspectives;Jul2004, Vol. 112 Issue 10, p1085 

    Polybrominated diphenyl ether (PBDE) congeners are constituents of flame retardants, and there is growing concern regarding their persistence, bioaccumulation, and toxicity. We collected breast milk samples between late 2001 and early 2003 from 54 U.K.-resident mothers. Of these, 27 originated...

Share

Read the Article

Courtesy of THE LIBRARY OF VIRGINIA

Sorry, but this item is not currently available from your library.

Try another library?
Sign out of this library

Other Topics