title: Liquid chromatography/tandem mass spectrometry for analysis of 1,2-dibromo-4-(1,2-dibromoethyl)cyclohexane (TBECH) and 1,2,5,6-tetrabromocyclooctane (TBCO).
abstract: Although the two flame retardants 1,2-dibromo-4-(1,2-dibromoethyl)cyclohexane (TBECH) and 1,2,5,6-tetrabromocyclooctane (TBCO) have been widely used, a selective instrumental method of analysis for these compounds has not been developed to date. In this study, we demonstrate the feasibility to utilize liquid chromatography/tandem mass spectrometry (LC/MS/MS) for the separation and analysis of α- and β-TBCO and α-, β-, γ-, and δ-TBECH. Acetone was initially used in a tetrahedron solvent system for LC optimization. A simple isocratic elution allowed near-baseline separation of these compounds. Different ionization approaches and mechanisms were investigated. The mass spectrometric transition of [M + O(2)](-) => Br(-) (459.8 => 78.9) was a selective detection method for the target analytes. Good instrument detection limits (5 pg for γ-/δ-TBECH, 125 pg for α-/β-TBECH, and 30 pg for α-/β-TBCO with 2.0 µL injection) were obtained. Excellent linearity up to 50 ng/µL (R(2) >0.999) was also achieved. This method has been applied to environmental samples (surface water) for screening purposes with recoveries ranging from 76-92% (CV%: 5-8%). This method shows significant improvement over previous methods.
authors.affiliation: Department of Chemistry, Brock University, St. Catharines, ON L2S 3A1, Canada. n3zhou@sciborg.uwaterloo.ca
authors.forename: Simon Ningsun
authors.initials: SN
authors.lastname: Zhou
authors.forename: Eric J
authors.initials: EJ
authors.lastname: Reiner
authors.forename: Chris H
authors.initials: CH
authors.lastname: Marvin
authors.forename: Paul A
authors.initials: PA
authors.lastname: Helm
authors.forename: Ian D
authors.initials: ID
authors.lastname: Brindle