Congener‐specific analysis of hexabromocyclododecane by high‐performance liquid chromatography/electrospray tandem mass spectrometry

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Abstract
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 C18 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.