The analytical performances of various adsorbents used to clean up an organic extract of biological samples, particularly for the determination of polycyclic aromatic hydrocarbons (PAHs), polychlorobiphenyls (PCBs), both in mussel tissue and in krill samples, are critically compared. DDT and its degradation products, namely DDE and DDD, are also considered. Silica gel, alumina, aminopropyl-silica, cyanopropyl-silica, florisil, graphitized nonporous carbon and silica gel–alumina mixture (3:1) were used for column chromatography cleanup in combination with modified supercritical CO2 as a mobile phase. Recovery and reproducibility were evaluated by analyzing standard solutions and standard reference materials containing various classes of pollutants. A silica gel–alumina mixture was found to be the most effective in the cleanup of organic extracts, allowing quantitative recoveries of all analytes to be obtained. Finally, the application of the optimized procedure to the determination of PCBs in Antarctic krill samples is presented.
Optimized cleanup methods of organic extracts for the determination of organic pollutants in biological samples
FUOCO, ROGER;GIANNARELLI, STEFANIA;CECCARINI, ALESSIO;
2005-01-01
Abstract
The analytical performances of various adsorbents used to clean up an organic extract of biological samples, particularly for the determination of polycyclic aromatic hydrocarbons (PAHs), polychlorobiphenyls (PCBs), both in mussel tissue and in krill samples, are critically compared. DDT and its degradation products, namely DDE and DDD, are also considered. Silica gel, alumina, aminopropyl-silica, cyanopropyl-silica, florisil, graphitized nonporous carbon and silica gel–alumina mixture (3:1) were used for column chromatography cleanup in combination with modified supercritical CO2 as a mobile phase. Recovery and reproducibility were evaluated by analyzing standard solutions and standard reference materials containing various classes of pollutants. A silica gel–alumina mixture was found to be the most effective in the cleanup of organic extracts, allowing quantitative recoveries of all analytes to be obtained. Finally, the application of the optimized procedure to the determination of PCBs in Antarctic krill samples is presented.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
