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A simplified method for determination of tetrabromobisphenol A and polybrominated diphenyl ethers in human plasma and serum
Author(s) -
Thomsen Cathrine,
Lundanes Elsa,
Becher Georg
Publication year - 2001
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/1615-9314(20010401)24:4<282::aid-jssc282>3.0.co;2-d
Subject(s) - chromatography , chemistry , tetrabromobisphenol a , polybrominated diphenyl ethers , derivatization , detection limit , solid phase extraction , diazomethane , extraction (chemistry) , elution , gas chromatography , high performance liquid chromatography , fire retardant , organic chemistry , pollutant
A method utilizing solid‐phase extraction (SPE) and gas chromatography with electron capture mass spectrometric detection (GC‐ECMS) has been developed for simultaneous determination of seven polybrominated diphenyl ethers (PBDEs) and tetrabromobisphenol A (TBBP‐A) in plasma and serum. Plasma and serum samples of 5.0 g were diluted and applied to a polystyrene‐divinylbenzene SPE column. The lipids were decomposed by treatment with concentrated sulfuric acid directly on the SPE column, prior to elution of the brominated flame retardants by dichloromethane‐methanol (7 + 3, v / v ). Following diazomethane derivatization, the samples were analyzed by GC‐ECMS. The method has been validated in the concentration range of 1.8–90 pg brominated flame retardants/g plasma or serum. The average absolute recoveries were in the range of 56–111% and 40–90% for plasma and serum, respectively. The average recoveries of the analytes relative to the internal standards were 75–108% and 88–111% for plasma and serum, respectively. The repeatability of the method was in the range of 0.6–27% RSD, and the estimated detection limits were in the range of 0.4–9.8 pg/g plasma or serum. The human plasma used for validation contained all the investigated analytes, in concentrations below 4 ng/g lipid weight.