Determination of PBDEs in human breast adipose tissues by gas chromatography coupled to triple quadrupole mass spectrometry
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Otros documentos de la autoría: Pitarch, Elena; Medina, Cecilia; Lopez, Francisco; Hernandez, Felix
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Mostrar el registro completo del ítemcomunitat-uji-handle:10234/9
comunitat-uji-handle2:10234/7013
comunitat-uji-handle3:10234/8638
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Título
Determination of PBDEs in human breast adipose tissues by gas chromatography coupled to triple quadrupole mass spectrometryFecha de publicación
2008Editor
Springer VerlagISSN
16182642Tipo de documento
info:eu-repo/semantics/articleVersión
info:eu-repo/semantics/acceptedVersionPalabras clave / Materias
Resumen
The potential of gas chromatography / tandem mass spectrometry with triple quadrupole
analyzer for determination of 12 polybrominated diphenyl ethers in human breast
tissues has been investigated. After extraction ... [+]
The potential of gas chromatography / tandem mass spectrometry with triple quadrupole
analyzer for determination of 12 polybrominated diphenyl ethers in human breast
tissues has been investigated. After extraction with hexane, two purification procedures
-automated normal-phase HPLC and solid phase extraction – were assayed. Both
electron impact ionization, in selected reaction monitoring mode, and negative chemical
ionization, in selected ion recording mode, were tested for the optimum determination
of analytes. Isotopically labelled standards were added before extraction as surrogates:
[13C] BDE47, [13C] BDE99 and [13C] BDE153 for EI, and p,p’-DDE-D8 for NCI.
The method was validated in terms of accuracy, precision, limits of detection and limits
of quantification, using human breast tissue spiked at three levels in the range 1-50 ng/g
(5-250 ng/g for BDE 209). The analytical approach using SPE clean-up followed by
GC-MS (NCI) led to lower detection limits (0.006-2 ng/g) and allowed the
determination of the most problematic congener, BDE 209, whose poor sensitivity made
difficult its determination at low residue levels. Special attention was given to the
confirmation of the compounds detected in samples in order to avoid reporting false
positives. Two MS/MS transitions or three m/z ions were selected for each analyte
when using EI or NCI modes, respectively. In both cases, the transition/ion intensity
ratio was used as confirmation parameter. The developed methodology was applied to
the analysis of real human samples. Several BDEs (BDEs congeners 47, 100, 99, 154,
153 183 and 209) were detected in the range of 0.08-0.23 ng/g [-]
Derechos de acceso
The original publication is available at www.springerlink.com
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info:eu-repo/semantics/openAccess
http://rightsstatements.org/vocab/InC/1.0/
info:eu-repo/semantics/openAccess
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