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Congener‐specific analysis of hexabromocyclododecane by high‐performance liquid chromatography/electrospray tandem mass spectrometry
Author(s) -
Budakowski Wesley,
Tomy Gregg
Publication year - 2003
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.1066
Subject(s) - chemistry , hexabromocyclododecane , chromatography , electrospray ionization , mass spectrometry , tandem mass spectrometry , analytical chemistry (journal) , electrospray , congener , selected reaction monitoring , detection limit , organic chemistry , fire retardant
A congener‐specific method based on high‐performance liquid chromatography/electrospray ionization tandem mass spectrometry (HPLC/ES‐MS/MS) in the negative ion mode was developed for the analysis of hexabromocyclododecane (HBCDD). On a C 18 analytical column, with a methanol/water mobile phase, the α ‐isomer was completely resolved from the β ‐ and γ ‐isomers while the β ‐ and γ ‐isomers were sufficiently resolved at half their peak heights. The ES spray voltage strongly influenced the intensity of the ion signal. For MS, a source temperature of 500°C and a collision energy of 50 eV were found to be optimum for the [M–H] − to Br − transition. Run‐to‐run and day‐to‐day (n = 3) variability was minimal, with relative standard deviations of 2.6–4.1 and 2.4–4.4%, respectively. The limit of detection was 4–6 pg on‐column. When applied to tissue samples from Lake Winnipeg fish both α ‐ and γ ‐isomers of HBCDD were found in low‐ng/g (lipid corrected) concentrations. Copyright © 2003 John Wiley & Sons, Ltd.