Development of a cleanup method for polybrominated diphenyl ether (PBDE) in fish by freezing-lipid filtration

Abstract

A new cleanup method for the determination of brominated flame retardants with an emphasis on polybrominated diphenyl ethers (PBDEs) has been developed for fish tissue sample. This method effectively reduces the sample pretreatment time, labor and required less solvent quantities relative to conventional methods. Freezing-lipid filtration procedure removes approximately 90 % of the lipids in the extract without any significant loss of the PBDEs. A multilayered silica gel column was used for further cleanup of the extracts after freezing-lipid filtration. Multilayered silica gel column chromatography eliminated most of the co-extracted interferences, such as residual lipids and fatty acids. The extracts were analyzed after cleanup by high-resolution gas chromatography/highresolution mass spectrometry using the isotope dilution method. Tissue samples with 1.6-8.0 and 8.0-40 ppb of PBDE were analyzed using both the sulfuric acid treatment and freezing-lipid filtration cleanup methods in order to evaluate the method performance. Sulfuric acid treatment did not detect 2,4-DiBDE, whereas freezing-lipid filtration detected 2,4-DiBDE but at 50 % recovery. To compare the method, WMF-01 was analyzed via both the sulfuric acid treatment and freezing-lipid filtration cleanup.

Removing Disturbing Matrix Constituents from Biota Extracts from Total Extraction and Silicone-Based Passive Sampling

“…antioxidants (log K OW (EPA) ranging from 0.56 for methylphenylsulfone to 12.26 for alpha-tocopherol acetate). In addition to the (i) Oasis PRiME and (ii) EMR-Lipid cartridges, we also tested the (iii) lipid freezing method (so-called "Freeze-Out") which can be adapted for small sample volumes and is widely used for the analysis of diverse chemicals in biota samples (Ahn 2006;Shin 2012;Desforges 2017;Álvarez-Ruiz 2020).…”

“…We selected 113 target chemicals covering pyrethroids, brominated diphenyl ethers (BDEs), polychlorinated biphenyls (PCBs), organochlorine pesticides (OCPs), substituted and nonsubstituted PAHs, musks, UV light filters, and antioxidants (log K OW [US Environmental Protection Agency 2000] ranging from 0.56 methyl phenyl sulfone to 12.26 alpha‐tocopherol acetate). In addition to the Oasis PRiME and EMR‐Lipid cartridges, we also tested the lipid freezing method, the so‐called “Freeze‐Out,” which can be adapted for small sample volumes and is widely used for the analysis of diverse chemicals in biota samples (Ahn et al 2006; Shin et al 2012; Desforges et al 2017; Álvarez‐Ruiz and Picó 2020). These methods were first tested with spiked total extracts of lipid‐rich salmon to evaluate compound recoveries and removal of unwanted lipid matrix constituents (extractable organic matter as a surrogate for lipids).…”

A Study on the TG/DTA Behavior of Decabromodiphenyl Ether

“…Many researchers have studied the analysis, determination and degradation methods of PBDEs [6,7]. Shin et al [8] developed a new cleanup method for the determination of BFRs with an emphasis on PBDEs of fish tissue sample. This method can effectively reduces the sample pretreatment time, labor and required less solvent quantities relative to conventional methods.…”