An automated HPLC method for the fractionation of polychlorinated biphenyls, polychlorinated dibenzo‐p‐dioxins, and polychlorinated dibenzofurans in fish tissue on a porous graphitic carbon column

Abstract

The Ah (aryl‐hydrocarbon) hydroxylase‐receptor active polychlorinated biphenyls (PCBs), polychlorinated dibenzo‐p‐dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) were fractionated by an automated high‐performance liquid chromatography (HPLC) system using the Hypercarb™ porous graphitic carbon (PGC) column. This commercially available column was used to fractionate the di‐, mono‐, and non‐ortho PCBs into three fractions for gas chromatography (GC)/electron capture detection analysis, and a fourth fraction containing the PCDDs/PCDFs for GC/mass spectrometry analysis. The recoveries of the PCBs ranged from 68 to 96%, and recoveries of the PCDDs/PCDFs ranged from 74 to 123%. The PGC column has the advantage of faster separations (110 min versus 446 min) and less solvent use (275 ml versus 1,100 ml) compared with automated fractionation of these compounds on activated carbon (PX‐21), while still affording good separation of the classes. The PGC column may have an advantage over the pyrenyl‐based HPLC method because it has a greater loading capacity (400 μg total PCBs versus 250 μg). Overall, the PGC is a standard column that provides reproducible fractionation of PCDD/PCDFs and PCBs for analytical measurement in environmental samples.

Dietary exposure of mink (Mustela vison) to fish from the Housatonic River, Berkshire County, Massachusetts, USA: Effects on reproduction, kit growth, and survival

“…All of the concentrated extracts were treated by a two‐stage reactive cleanup, and residual lipids were removed by high‐pressure gel permeation chromatography [17]. Aliquots of these extracts were fractionated with the use of high‐performance porous graphite carbon chromatography according to the procedures in Echols et al [19]. The instrument analysis for the determination of the congener‐specific PCBs (fraction 1) was as described above by GC/ECD.…”

Dietary exposure of mink (Mustela vison) to fish from the Housatonic River, Berkshire County, Massachusetts, USA: Effects on organ weights and histology and hepatic concentrations of polychlorinated biphenyls and 2,3,7,8-tetrachlorodibenzo-p-dioxin toxic equivalence

“…All the concentrated extracts were treated by a two-stage reactive cleanup, and residual lipids were removed by high-pressure gel permeation chromatography [18]. Aliquots of these extracts were then fractionated using high-performance porous graphite carbon chromatography according to the procedures described by Echols et al [20]. The instrument analysis for the determination of the congener-specific PCBs (fraction 1) was as described above by gas chromatography with electron-capture detection.…”

Turtle sex determination assay: Mass balance and responses to 2,3,7,8‐tetrachlorodibenzo‐p‐dioxin and 3,3′,4,4′,5‐pentachlorobiphenyl

“…For the pooled eggshell samples with expected high concentrations of PHHs, no further cleanup was performed. For the pooled tissue samples, the non‐ ortho ‐PCB and polychlorinated dibenzo‐ p ‐dioxin and dibenzofuran (PCDD/DF) fractions, containing PCB‐126 and TCDD, respectively, were separated by highperformance carbon chromatography [34]. The PCDD/DF fractions were eluted through basic alumina to remove potential interferences.…”

“…The PCDD/DF fractions were eluted through basic alumina to remove potential interferences. The chemicals of interest were quantified using capillary gas chromatography with high‐resolution isotope dilution mass spectrometry [34,35].…”