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Determination of ten hexabromocyclododecane diastereoisomers using two coupled reversed‐phase columns and liquid chromatography/tandem mass spectrometry
Author(s) -
Han Qian,
Song Han,
Gao Shutao,
Zeng Xiangying,
Yu Zhiqiang,
Yu Yunjiang,
Sheng Guoying,
Fu Jiamo
Publication year - 2014
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.6922
Subject(s) - chemistry , diastereomer , hexabromocyclododecane , chromatography , tandem mass spectrometry , electrospray ionization , mass spectrometry , liquid chromatography–mass spectrometry , selected reaction monitoring , electrospray , enantiomer , organic chemistry , fire retardant
RATIONALE Hexabromocyclododecanes (HBCDs) are raising concern due to their potential persistence, bioaccumulation and toxicity. Apart from the widely reported isomers α‐, β‐, γ‐HBCD, other HBCD diastereoisomers such as δ‐HBCD have been also recently found in environmental media and biota. These newly reported diastereoisomers might give more insight into the degradation and biotransformation of HBCDs. METHODS A reversed‐phase C 18 column coupled to a C 8 column was used to improve the chromatographic resolution. A gradient mobile phase consisting of methanol, acetonitrile, and water, as well as tandem mass spectrometry parameters, were optimized. Ten HBCD diastereoisomers were finally determined by liquid chromatography/tandem mass spectrometry in multiple reaction monitoring mode with negative electrospray ionization. RESULTS Eight of the ten HBCDs could be chromatographically separated by using the coupled reversed‐phase columns. Results of the method validation indicate high reproducibility and good sensitivity. The limit of detection ranged from 0.4 to 0.8 pg, and the relative standard deviations of intra‐ and inter‐day injections ranged from 1.8 to 5.1% and from 2.7 to 9.5%, respectively. The developed method was further applied to the analysis of HBCDs in HBCD commercial products and soil samples. δ‐, η‐, θ‐, and ε‐HBCD were detected in commercial products and soil samples. CONCLUSIONS The present study revealed that δ‐, η‐, θ‐, and ε‐HBCD might occur ubiquitously in environmental media and biota. These newly reported diastereoisomers may help us to better understand the fate and transformation of HBCDs in the environment. Copyright © 2014 John Wiley & Sons, Ltd.