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Liquid chromatography/tandem mass spectrometry for analysis of 1,2‐dibromo‐4‐(1,2‐dibromoethyl)cyclohexane (TBECH) and 1,2,5,6‐tetrabromocyclooctane (TBCO)
Author(s) -
Zhou Simon Ningsun,
Reiner Eric J.,
Marvin Chris H.,
Helm Paul A.,
Brindle Ian D.
Publication year - 2011
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.4878
Subject(s) - chemistry , chromatography , mass spectrometry , cyclohexane , analyte , tandem mass spectrometry , elution , detection limit , solvent , analytical chemistry (journal) , organic chemistry
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. Copyright © 2011 John Wiley & Sons, Ltd.