English   español  
Please use this identifier to cite or link to this item: http://hdl.handle.net/10261/191868
logo share SHARE logo core CORE   Add this article to your Mendeley library MendeleyBASE

Visualizar otros formatos: MARC | Dublin Core | RDF | ORE | MODS | METS | DIDL | DATACITE
Exportar a otros formatos:


Miniaturised sample preparation of fatty foodstuffs for the determination of polychlorinated biphenyls

AuthorsRamos, Juan José ; González, María José; Ramos, Lourdes
Issue Date2004
CitationJournal of Separation Science 27(7-8): 595-601 (2004)
AbstractA miniaturised analytical method allowing the exhaustive extraction of environmentally relevant polychlorinated biphenyls (PCBs) from fatty foodstuffs and the purification of the extracts in a single step has been developed. After dispersion of the freeze dried sample on silica modified with 44% (w/w) of sulphuric acid, the mixture was packed in a glass column on top of a multilayer silica column used for removal of the lipids and biogenic co-extracted material. Using this arrangement, a complete sample preparation can be accomplished by two successive 10 min static extractions with hexane followed by a brief dynamic step to ensure purging of the sample and sorbents. The analytical method showed a satisfactory performance, with recoveries of the endogenous PCBs studied in the 81-134% range of those found using a more conventional off-line procedure, even though as small an amount of sample as 0.1 g was used. Detection limits by gas chromatography with micro-electron capture detection (GC-ECD) were in all cases lower than 0.3 ng/g sample (freeze dried basis) and the repeatability of the complete analytical procedure better than 14% (except for PCB 167). When combined with GC and ion trap detection in the tandem mass spectrometry mode, the miniaturised method has been proved to be a valuable alternative to the more expensive high resolution mass spectrometry for fast screening of PCBs 77, 126, and 169, even if these congeners were not isolated from the bulk of PCBs.
Publisher version (URL)https://doi.org/10.1002/jssc.200301648
Appears in Collections:(IQOG) Artículos
Files in This Item:
File Description SizeFormat 
accesoRestringido.pdf59,24 kBAdobe PDFThumbnail
Show full item record
Review this work

WARNING: Items in Digital.CSIC are protected by copyright, with all rights reserved, unless otherwise indicated.