A new method for determination of halogenated flame retardants in human milk using solid-phase extraction.
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.
Thomsen
Cathrine
C
National Institute of Public Health, Oslo, Norway. cathrine.thomsen@folkehelsa.no
Leknes
Henriette
H
Lundanes
Elsa
E
Becher
Georg
G
D005260:Female; D005411:Flame Retardants / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D006846:Hydrocarbons, Halogenated / Q000032:analysis*; D008895:Milk, Human / Q000737:chemistry*; D009664:Norway; D011075:Polybrominated Biphenyls / Q000032:analysis; D015203:Reproducibility of Results
D005411:Flame Retardants; D006846:Hydrocarbons, Halogenated; D011075:Polybrominated Biphenyls