Abstract
We have previously described the use of a tandem simplified multilayer silica gel-activated carbon dispersed silica gel (TS-ML-AC) column for the cleanup of blood samples for the analysis of 29 hazardous organochlorine compounds (OCs)--the 17 major polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDDs/DFs) and 4 non-ortho- and 8 mono-ortho-polychlorinated biphenyls (PCBs). We noted that the performance of the activated carbon-silica gel (ACS) column (lower column) varied with the lot number of the ACS. In this study, we compared the elution profiles of OCs eluted on 5 ACS columns, each with a different ACS lot number, and found that only mono-ortho-PCBs #114 and #123 were affected by lot number. The problem was that the 50 ml of n-hexane required to elute all the OCs from the simplified multilayer silica gel (MLS) column (upper column) into the AC column (lower column) also eluted varying amounts of PCBs #114 and #123 from the ACS column by ACS lot number. Although we could prevent PCBs #114 and #123 from being eluted from the ACS column by reducing the n-hexane volume to 10 ml, this volume was not sufficient to elute all the OCs from the MLS column. We solved this by separating the two columns; the sample solution was eluted with 50 ml of n-hexane from the MLS column, this eluate was concentrated to about 0.3 ml using a rotary evaporator, and then the concentrated solution was cleaned up on the ACS column. The recovery rates of #114 and #123 from blood samples were above 70% and the relative standard deviations of their concentration were below 10%, irrespective of the lot number, compared with recovery rates of 45-79% for #114 and 59-89% for #123, and relative standard deviations of their concentration above 15% when 50 ml of n-hexane was run through the tandem column. Our modified method affords reliable and reproducible cleanup of blood samples for analysis of 29 OCs, irrespective of the ACS lot number.
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