Cited by 40Analytical chemistry methods developmentToxic Organic Pollutants ImpactPesticide Residue Analysis and Safety

Determination of polybrominated diphenyl ethers in aquatic animal tissue using cleanup by freezing‐dispersive liquid–liquid microextraction combined with GC‐MS

Liu, Xiujuan, Hu, Jia, Huang, Changjiang, Wang, Huili, Wang, Xuedong·2009·Journal of Separation Science

Abstract

A method for the determination of polybrominated diphenyl ethers (PBDEs) in aquatic animal tissue was developed, and it is based on cleanup by freezing-dispersive liquid-liquid microextraction (DLLME) for the pretreatment of samples with fat content. Aquatic animal tissue homogenate was extracted with acetone, and then frozen in a freezer at -80 degrees C. Fat in aquatic animal tissue was isolated from the analytes, i.e. PBDE congeners dissolved in acetone and fat formed floccules at low temperature. The supernatant was extracted using the DLLME technique. Under the optimum DLLME conditions, 0.75 mL supernatant with 33 microL chlorobenzene was added into 5.0 mL pure water, and subsequently cloudy solution was formed. After centrifuging, 1.0 microL lower phase was subjected to GC-MS analysis. Recovery test was performed at fortified concentrations of 5.0-2500 microg/kg. The detection results showed that the recoveries for each target analyte ranged from 75.3 to 127.8%. The repeatability of the proposed method by spiking aquatic animal samples at 10 microg/kg for PBDEs, expressed as RSD, n=5, varied between 4.3 and 10.3% (n=5). LOD of the proposed method for aquatic animal tissue samples were between 2.4 and 4.9 microg/kg for all the analytes.

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Crossref · 10.1002/jssc.200900480

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  • Only on a few occasions were complex samples analyzed for PCBs/PBDEs, such as soils or aquatic organisms.

    “From Table 3, it is clear that only on a few occasions were there analyses of complex samples {e.g., soils [60] or aquatic organisms in which bioaccumulation of these analytes may occur [59,61]}.”
  • Chlorobenzene and tetrachloroethane were preferred as extractant solvents for PCBs/PBDEs, while acetonitrile and acetone were used as disperser solvents, except one case using tetrahydrofurane.

    “Chlorobenzene [59-61,77] and tetrachloroethane [56,76,78] were preferred in all cases as extractant solvents (volumes less than 35 l L), while acetonitrile [56,76] and acetone [5961,77] were used as disperser solvent, except in one case in which tetrahydrofurane was used [78].”
  • The LODs for Liu et al. [61] were 2.4-4.9 μg/kg.

    “The LODs were slightly higher (2.4-4.9 l g/kg).”
  • So far, DLLME has been used for determination of PCBs by HPLC-UV and PBDEs by GC-ECD and GC-MS.

    “So far, the technique has been used for the determination of PCBs by HPLC-UV [76-78] and PBDEs by GC-ECD [56,59,60,72] and GCMS [61].”
  • Liu et al. [61] applied the same method to determine PBDEs in frog, snail and fish.

    “Later, Liu et al. [61] applied the same method to determine PBDEs in frog, snail and fish using 4 g of anhydrous Na2SO4, 33 l L of chlorobenzene and 0.75 mL of acetone extract.”

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Authors
Liu, X., Hu, J., Huang, C., Wang, H., & Wang, X.
Affiliations
  • Wenzhou Medical University (CN)
  • Central China Normal University (CN)
Corresponding author
  • Huang, Changjiang
  • Wang, Xuedong
Venue
Journal of Separation Science
Publisher
Wiley
Published
2009-12
Volume
32
Issue
23-24
Pages
4213-4219
ISSN
  • 1615-9306 (ISSN-L)
  • 1615-9314
OpenAlex
W2143295139
Cited by
40
References
35
Citations by year
2026: 1 · 2025: 1 · 2024: 1 · 2022: 3 · 2020: 2 · 2019: 3 · 2018: 3 · 2017: 1 · 2016: 5 · 2015: 2 · 2014: 3 · 2013: 1 · 2012: 5
FWCI
4.54
Type
journal article
Language
en
Open access
closed
Locations
  • Journal of Separation Science (publishedVersion)
  • PubMed (publishedVersion)
Funders
  • Key Project of Natural Science Foundation of Zhejiang Province (Z2080266)
  • Analyzing and Testing Foundation of Zhejiang Province (2008F70062)
  • International Cooperation Project of Wenzhou City (H20090023, H20080063)
  • Best Management Practice (20082780125)
Topics
  • Physical Sciences › Chemistry › Analytical Chemistry › Analytical chemistry methods development
  • Physical Sciences › Environmental Science › Health, Toxicology and Mutagenesis › Toxic Organic Pollutants Impact
  • Life Sciences › Agricultural and Biological Sciences › Food Science › Pesticide Residue Analysis and Safety
Keywords
polybrominated diphenyl ethers, PBDE congeners, sample cleanup, fat removal, brominated flame retardants, environmental pollutants, sample preparation
MeSH terms
Animals, Environmental Pollutants, Fishes, Flame Retardants, Freezing, Gas Chromatography-Mass Spectrometry, Ranidae, Snails, Solvents, Halogenated Diphenyl Ethers

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