Quantitative analysis of polybrominated diphenyl ethers in adipose tissue, human serum and foodstuff samples by gas chromatography with ion trap tandem mass spectrometry and isotope dilution.
A method based on gas chromatography (GC) separation followed by ion trap tandem mass spectrometry detection in EI mode (ITD-MS/MS), using isotope dilution, was developed for the determination of ten native polybrominated diphenyl ethers (PBDEs) and four (13)C(12)-labeled congeners in biological (fat tissue and human serum) and food samples. The highest-mass fragment ions were used as precursor ions for those congeners with molecular ions with m/z values higher than the maximum of the instrument. In these cases (hepta-BDEs and (13)C(12)-hexa-BDEs) no fragmentation was achieved under the experimental conditions employed. Repeatability (lower than 9%) and reproducibility (lower than 13%), expressed as relative standard deviation (RSD, n = 3 and 4, respectively), were satisfactory. Similarly, the coefficient of variation (n = 4) of the isotopic ratio between the two most abundant product ions was lower than 10 and 6% for native and labeled congeners, respectively. To evaluate the feasibility of the method, the optimized isotope dilution GC/ITD-MS/MS method was used for the quantitation of selected PBDE congeners in different samples including adipose tissue, human serum and foodstuff samples, from three inter-laboratory comparative exercises, covering a wide range of concentrations. A solid-phase extraction procedure, previously developed for PCB determination in small-size bird serum samples, was successfully applied to quantification of PBDEs in 1 mL samples of human serum.
Gómara
Belén
B
Department of Instrumental Analysis and Environmental Chemistry, IQOG (CSIC), Juan de la Cierva 3, 28006 Madrid, Spain.
Herrero
Laura
L
Bordajandi
Luisa R
LR
González
María José
MJ
D000273:Adipose Tissue / Q000737:chemistry*; D000818:Animals; D001774:Blood Chemical Analysis / Q000379:methods*; D002849:Chromatography, Gas / Q000379:methods*; D004785:Environmental Pollutants / Q000032:analysis; D004987:Ethers / Q000032:analysis; D005240:Feasibility Studies; D005504:Food Analysis / Q000379:methods*; D006801:Humans; D011075:Polybrominated Biphenyls / Q000032:analysis*; D011865:Radioisotope Dilution Technique; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013048:Specimen Handling / Q000379:methods; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
D004785:Environmental Pollutants; D004987:Ethers; D011075:Polybrominated Biphenyls