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

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.