Analysis of Hexabromocyclododecane Diastereomers and Enantiomers by Liquid Chromatography Tandem Mass Spectrometry: Chromatographic Selectivity and Ionization Matrix Effects

Published

October 2, 2006

Author(s)

Nathan G. Dodder, Aaron Peck, John R. Kucklick, Lane C. Sander

Abstract

Hexabromocyclododecane (HBCD) is a flame retardant that is undergoing environmental risk assessment. The liquid chromatographic retention and electrospray ionization matrix effects were investigated for HBCD methods of analysis for environmental matrices. Column selectivity towards HBCD diastereomers was evaluated for C30 and C18 stationary phases under different mobile phase conditions and column temperatures. The HBCD elution order was dependent on the shape selectivity of the stationary phase and the mobile phase composition. Greater resolution of B-HBCD and y-HBCD was achieved with the use of an acetonitrile / water (compared with a methanol / water) mobile phase composition. A liquid chromatography / electrospray ionization tandem mass spectrometry (LC / ESI-MS/MS) method for the analysis of HBCD in biological tissues was evaluated for potential matrix effects. The influence of extracted matrix components on HBCD diastereomer and enantiomer analysis was investigated using a postextraction addition approach. Although the analysis of HBCD diastereomers was relatively unaffected by the sample matrix, HBCD enantiomers in tissue samples were significantly influenced by extracted matrix components. The use of racemic 13C-labeled HBCD diastereomers as internal standards for enantiomer fraction measurements corrected for the changes in the mass spectrometer response.

Citation

Journal of Chromatography A

Volume

1135

Issue

1

Pub Type

Journals

Download Paper

Local Download

Keywords

electrospray ionization, enantiomer fraction, hexabromocyclododecane, liquid chromatography, matrix effects, shape selectivity, stable isotope internal standard, tandem mass spectrometry

Citation

Dodder, N. , Peck, A. , Kucklick, J. and Sander, L. (2006), Analysis of Hexabromocyclododecane Diastereomers and Enantiomers by Liquid Chromatography Tandem Mass Spectrometry: Chromatographic Selectivity and Ionization Matrix Effects, Journal of Chromatography A, [online], https://tsapps.nist.gov/publication/get_pdf.cfm?pub_id=832119 (Accessed January 15, 2025)