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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 26, Number 3, April,
pp. 129-138
A New Method for Determination of Halogenated Flame Retardants
in Human Milk Using Solid-Phase Extraction
Cathrine Thomsen[1], Henriette Leknes[1], Elsa
Lundanes[2], and Georg Becher[1],[2]
[1]National Institute of Public Health, P.O. Box 4404 Nydalen, N-0403 Oslo,
Norway and
[2]Department of Chemistry, University of Oslo, P.O. Box 1033 Blindern, N-0315
Oslo, Norway
A method has been developed
for quantitation of a selection of halogenated flame retardants in human milk.
The method has been validated for seven polybrominated diphenyl ethers (PBDEs),
BDE-28, BDE-47, BDE-99, BDE-100, BDE-153, BDE-154, and BDE-183, and the halogenated
phenols 2,4,6-tribromophenol (TriBP), pentabromophenol (PeBP), tetrachlorobisphenol-A
(TCBP-A), and tetrabromobisphenol-A (TBBP-A). The sample preparation includes
solid-phase extraction using an N-vinylpyrrolidone-divinylbenzene copolymer
with on-column lipid decomposition followed by additional cleanup on sulfuric
acid-silica columns and methylation of the phenolic compounds. Separation and
detection were performed by gas chromatography–electron capture mass spectrometry,
using a 5% phenyl 95% dimethylpolysiloxane column. The method has been validated
in the range of 1.8–180 pg/g milk for most of the halogenated flame retardants.
The average absolute recoveries were from 49 to 83%, and the average recoveries
with respect to internal standards were in the range of 53 to 121%. Estimated
limits of detection were in the range of 0.3 to 1.0 pg/g milk using a sample
size of 5 g for all compounds, except TCBP-A, for which the limit of detection
was estimated to 6.7 pg/g milk. Reproduction
of editorial content of this journal is prohibited without publisher’s
permission.
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