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Miniaturized selective pressurized liquid extraction of polychlorinated biphenyls and polybrominated diphenyl ethers from feedstuffs

AuthorsPena-Abaurrea, Miren; Ramos, Juan José ; Gonzalez, María José; Ramos, Lourdes
KeywordsSelective pressurized liquid extraction
Feed analysis
Issue Date2013
CitationJournal of Chromatography A 1273: 18-25 (2013)
AbstractA new miniaturized pressurized liquid extraction (PLE) with in-cell purification method has been developed for the simultaneous extraction of endogenous prioritary and toxic polychlorinated biphenyls (PCBs) and environmentally relevant tri- to deca-brominated diphenyl ether (PBDE) congeners from different feed matrices. Parameters affecting the efficiency of the selective PLE process, such as sorbent:matrix ratio, volume and nature of the extraction solvent, PLE working mode, extraction time and temperature, and amount of co-sorbents, were optimized. n-Hexane and n-hexane:dichloromethane (1:1, v/v) were used as extraction solvents. 8-mL of organic solvents and 3.5. g of sorbents sufficed for complete sample treatment. Only 0.25. g of feed sample were required for accurate determination of the endogenous PCBs studied using gas chromatography with a micro-electron capture detector (GC-οECD) during method development, and for PBDE analysis using either GC-οECD or gas chromatography with negative chemical ionization-quadrupole mass spectrometry (GC-NCI-qMS). Gas chromatography coupled to ion trap detection working in tandem mode, GC-ITD (MS/MS), was used for final PCB confirmation. Additional purification of the sample extracts was not required. The performance of the complete PLE-based method was evaluated at two spiking levels, 0.4 and 4. ng/g wet weight. Recoveries in the range 60-120% were obtained for PCBs, while those of PBDEs ranged from 86% to 114% for most of the target analytes. The relative standard deviations were in general lower than 20%. The optimized procedure was applied to the determination of the investigated PCBs and PBDEs in a variety of feed samples.
Identifiersdoi: 10.1016/j.chroma.2012.11.066
issn: 0021-9673
e-issn: 1873-3778
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