Determination of Polybrominated Diphenyl Ethers in Baiyang Lake by Dispersive Liquid-Liquid Microextraction and Gas Chromatography/Gas Chromatography-Mass Spectrometry

2010 
Dispersive liquid-liquid microextraction(DLLME) is a very simple and rapid method for the extraction and preconcentration of polybrominated diphenyl ethers (PBDEs) in water samples. Approximately 42 PBDEs were extracted by DLLME and determinated by gas chromatography coupled with the micro-electron capture detector (GC-mu ECD) and gas chromatography-mass spectrometry. In this method, the mixture of chlorobenzene(25 p,L) and acetonitrile (1.0 mL) were injected into samples rapidly, then centrifugated for 15 min at 3000 r/min, after that the organic phase was drawn from the centrifuge tube and evaporated to dryness by nitrogen. The residue was dissolved by 17 ill, acetone, and 1 mu L was injected into the GC. Under the optimized conditions, PBDEs can be extracted completely and separated well. Good linear relationships were obtained in the concentrations of 2.0 - 250.0 mu g/L of the analyte with the correlation coefficients of 0.9982 - 0.9999. The limits of detection were between 0.2 and 4.9 ng/L(S/N = 3). The water samples collected from Baiyang Lake were successfully analyzed using the proposed method. BDE-166 and BDE-209 were detected in all water samples. The recoveries, which had been spiked with different levels (0.017 and 0.170 mu g/L), fell in the range of 71.4% - 110.8% and the relative standard deviations were between 1.0% and 11.9% (n = 3). The results showed that the proposed method would be valuable for PBDEs analysis in environmental water samples.
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