期刊
JOURNAL OF SEPARATION SCIENCE
卷 34, 期 9, 页码 1084-1090出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.201000767
关键词
GC-MS; Milk sample; Polybrominated diphenyl ethers (PBDEs); Polychlorinated biphenyls (PCBs); SPE combined with dispersive liquid-liquid microextraction
资金
- International Cooperation Project of Wenzhou City [H20090079, H20090080, S20100034]
- Analyzing and Testing Foundation of Zhejiang Provine [2009F70045]
- Health Bureau of Zhejiang Province [2009A136]
An effective multi-residue pretreatment technique, solid-phase extraction (SPE) combined with dispersive liquid-liquid microextraction (DLLME), was proposed for the trace analysis of 14 polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) in milk samples using gas chromatography-mass spectrometry (GC-MS). Interesting analytes in milk samples were extracted with hexane after protein precipitation. The hexane extracts were loaded on an LC-Florisil column to isolate analytes from the milk matrix. The elutes were dried and dissolved in acetone, which was used as the disperser solvent in subsequent DLLME procedures. The effects of several important parameters on the extraction efficiency were evaluated. Under the optimized conditions, a linear relationship was obtained in the range of 0.02-10.00 mu g/L (PCBs) and 0.5-100.00 mu g/L (PBDEs). The LOD (S/N=3) and relative standard deviations (RSDs, n=5) for all analytes were 0.01-0.4 mu g/L and 0.6-8.5%, respectively. The recoveries of the standards added to raw bovine milk samples were 74.0-131.8%, and the repeatabilities of the analysis results were 1.12-17.41%. This method has been successfully applied to estimating PCBs and PBDEs in milk samples.
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