Determination of polybrominated diphenyl ethers in aquatic animal tissue using cleanup by freezing‐dispersive liquid–liquid microextraction combined with GC‐MS
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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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]}.”
From Dispersive liquid-liquid microextraction for determination of organic analytes (2010) · cites this paper as [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].”
From Dispersive liquid-liquid microextraction for determination of organic analytes (2010) · cites this paper as [61]
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).”
From Dispersive liquid-liquid microextraction for determination of organic analytes (2010) · cites this paper as [61]
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].”
From Dispersive liquid-liquid microextraction for determination of organic analytes (2010) · cites this paper as [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.”
From Dispersive liquid-liquid microextraction for determination of organic analytes (2010) · cites this paper as [61]
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References 35 · Cited by 40
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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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