Factorial-design optimization of gas chromatographic analysis of tetrabrominated to decabrominated diphenyl ethers. Application to domestic dust |
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Authors: | Jorge Regueiro Maria Llompart Carmen Garcia-Jares Rafael Cela |
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Institution: | (1) Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis de Alimentarios, Universidad de Santiago de Compostela, 15782 Santiago de Compostela, Spain |
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Abstract: | Gas chromatographic analysis of polybrominated diphenyl ethers (PBDEs) has been evaluated in an attempt to achieve better
control of the separation process, especially for highly substituted congeners. Use of a narrow-bore capillary column enabled
adequate determination of tetra, penta, hexa, hepta, octa, nona and decaBDE congeners in only one chromatographic run while
maintaining resolution power similar to that of conventional columns. A micro electron-capture detector (GC–μECD) was used.
Chromatographic conditions were optimized by multifactorial experimental design, with the objective of obtaining not only
high sensitivity but also good precision. In this way two different approaches to maximizing response and minimizing variability
were tested, and are fully discussed. These optimum chromatographic conditions were then used to determine PBDEs extracted
from domestic dust samples by microwave-assisted solvent extraction (MASE). Quantitative recovery (90–108%) was achieved for
all the PBDEs and method precision (RSD < 13%) was satisfactory. Accuracy was tested by use of the standard reference material
SRM 2585, and sub-ng g−1 limits of detection were obtained for all compounds except BDE-209 (1.44 ng g−1). Finally, several samples of house dust were analysed by use of the proposed method and all the target PBDEs were detected
in all the samples. BDE-209 was the predominant congener. Amounts varied from 58 to 1615 ng g−1 and the average contribution to the total PBDE burden of 52%. The main congeners of the octaBDE mixture (BDE-183, BDE-197,
BDE-207 and BDE-196) also made an important contribution (29%) to the total. These are the first data about the presence of
these compounds in European house-dust samples. Finally, the sum of the main congeners in the pentaBDE commercial mixture
(BDE-47, BDE-99, and BDE-100) contributed 14% to the total.
Figure Polybrominated diphenyl ethers in House Dust |
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Keywords: | Polybrominated diphenyl ethers Flame retardants Factorial design Gas chromatography– μ ECD Microwave-assisted solvent extraction House dust |
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