期刊
JOURNAL OF SEPARATION SCIENCE
卷 34, 期 9, 页码 1047-1054出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.201000631
关键词
Beverage; Dispersive liquid-liquid microextraction; Dispersive solidphase extraction; GC-MS; Polybrominated diphenyl ethers
资金
- National Natural Science Foundation of China [20605021, 20975099]
- Key Projects in the National Science and Technology Pillar Program during the Eleventh Five-Year Plan Period [2009ZX09308-006-5]
- Research Subjects in the National Science and Technology Innovative Plan [2010IM030400]
A simple, inexpensive and reliable analytical method was developed for the determination of polybrominated diphenyl ethers (PBDEs) in polyethylene terephthalate (PET) bottled beverage using GC-MS. The sample pretreatment using dispersive solid-phase extraction (DSPE) for removing matrix and dispersive liquid-liquid microextraction (DLLME) for enriching analytes was performed. For the DSPE, different sorbents such as primary amine, secondary amine, C-18 and graphitized carbon black were tested for different sample matrices. By means of DSPE, 60-89% of the sample matrices could be removed. Acetonitrile solution obtained by DSPE cleanup was directly used as the dispersant for the subsequent DLLME, which made the combination of the DSPE with the DLLME much more straightforward. Under the optimal conditions, the enrichment factors (EFs) of PBDEs ranged from 199 to 292. Using matrix-matched calibration, correlation coefficients above 0.994 were found and LODs ranged from 0.0023 to 0.15 mu g/L. The recoveries were between 80 and 117% for beverages spiked at three different concentrations (1.0, 5.0 and 10 mu g/L) with RSDs ranging from 3.7 to 14.7% (n=5). The results indicated that the combination of DSPE with DLLME was a powerful sample preparation tool for analysis of ultratrace analytes in complicated matrices.
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