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GC‐MS/MS multi‐residue method for the determination of organochlorine pesticides, polychlorinated biphenyls and polybrominated diphenyl ethers in human breast tissues
Author(s) -
Medina Cecilia M.,
Pitarch Elena,
Portolés Tania,
López Franciso J.,
Hernández Félix
Publication year - 2009
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/jssc.200800737
Subject(s) - chemistry , polybrominated diphenyl ethers , chromatography , analyte , detection limit , triple quadrupole mass spectrometer , selected ion monitoring , residue (chemistry) , diphenyl ether , chemical ionization , gas chromatography , gas chromatography–mass spectrometry , environmental chemistry , mass spectrometry , selected reaction monitoring , tandem mass spectrometry , ionization , ion , organic chemistry , pollutant
In this work, a multiresidue method for the quantification and confirmation of around 30 organohalogenated compounds in human breast tissue samples has been developed. Analytes tested included organochlorine (OC) (pesticides and polychlorinated biphenyls) and organobromine (OBr) (polybrominated diphenyl ether) compounds. The approach is based on a simple extraction with hexane, followed by a SPE clean‐up using silica cartridges and final measurement by GC coupled to triple quadrupole MS. Analyses were performed in both ionizations, electron impact (EI) (selected reaction monitoring (SRM) mode) and negative chemical ionization (NCI) (selected ion recording (SIR) mode). Three isotopically labeled standards were added before extraction and used as surrogates: HCB‐ 13 C 6 , lindane‐D 6 and p,p ′‐DDE‐D 8 . The method was validated in terms of accuracy, precision, LOQ and LOD and confirmation reliability, using breast tissue spiked at three concentration levels in the range 1–100 ng/g for OC compounds and at two levels 0.1 and 10 ng/g for OBr compounds (0.5 and 50 ng/g for BDE 209). The usefulness of the developed method was tested by the analysis of real human samples, giving as a result the detection of several OC and OBr compounds in different samples analyzed. The acquisition of at least two SRM transitions (in EI) or ions (in NCI) per analyte allowed positive findings to be confirmed by accomplishment of ion ratios between the quantification and the confirmation transitions or ions.