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Analysis of hydroxylated polybrominated diphenyl ethers (OH-BDEs) by supercritical fluid chromatography/mass spectrometry

Gross, Michael S., Olivos, Hernando J., Butryn, Deena M., Olson, James R., Aga, Diana S.
Talanta 2016 v.161 pp. 122-129
biochemical compounds, blood serum, derivatization, detection limit, gas chromatography-mass spectrometry, humans, liquid chromatography, metabolism, neurotoxicity, polybrominated diphenyl ethers, risk, supercritical fluid chromatography, wildlife
Hydroxylated polybrominated diphenyl ethers (OH-BDEs), which have anthropogenic and natural origins, have exhibited neurotoxic and endocrine disrupting effects in humans and wildlife. Therefore, there is an increased interest in the analysis of these compounds in biological matrices in order to assess their potential toxicological risks. Analysis of OH-BDEs is conventionally completed using liquid chromatography/mass spectrometry (LC/MS), or by gas chromatography/mass spectrometry (GC/MS) after derivatization. Issues with resolution in separating congeners have limited the analysis of OH-BDEs via LC/MS, with published methods only able to include 13 congeners in the analysis. On the other hand, while GC/MS analysis can analyze more OH-BDE congeners, derivatization of OH-BDEs to convert them to GC amenable compounds adds to sample preparation time and limits the column lifetime due to trace residues of highly reactive derivatization agents entering the column. Herein we report the development of a supercritical fluid chromatography/mass spectrometry (SFC/MS) method for the analysis of 22 OH-BDE congeners. Instrument limits of detection for the developed method ranged from 2 to 106fg injected on column, which is lower than previously optimized LC/MS and GC/MS methods. The developed SFC/MS method was successfully applied towards the analysis of in vitro metabolism samples and human serum samples to demonstrate its applicability with different biological matrices.