期刊
JOURNAL OF SEPARATION SCIENCE
卷 32, 期 23-24, 页码 4213-4219出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.200900480
关键词
Aquatic animal tissue; Cleanup by freezing-dispersive liquid-liquid microextraction; GC-MS; Polybrominated diphenyl ethers
资金
- 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 (BMP) Project of Wenruitang River of Wenzhou City [20082780125]
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 mu L chlorobenzene was added into 5.0 mL pure water, and subsequently cloudy solution was formed. After centrifuging, 1.0 mu L lower phase was subjected to GC-MS analysis. Recovery test was performed at fortified concentrations of 5.0-2500 mu g/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 mu g/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 mu g/kg for all the analytes.
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