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 alpha-isomer was completely resolved from the beta- and gamma-isomers while the beta- and gamma-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 degrees 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 alpha- and gamma-isomers of HBCDD were found in low-ng/g (lipid corrected) concentrations.
Budakowski
Wesley
W
Department of Fisheries and Oceans, 501 University Crescent, Winnipeg, MB R3T 2N6, Canada.
Tomy
Gregg
G
D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005399:Fishes; D005411:Flame Retardants / Q000032:analysis; D006842:Hydrocarbons, Brominated / Q000032:analysis* / Q000737:chemistry*; D007536:Isomerism; D018482:Muscle, Skeletal / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
D005411:Flame Retardants; D006842:Hydrocarbons, Brominated; C089796:hexabromocyclododecane