Analysis of a Mixture of Polychlorinated Biphenyls and Chlorinated Pesticides in Human Serum by Column Fractionation and Dual-Column Capillary Gas Chromatography with Electron Capture Detection

Abstract

An analytical method is presented for precise identification and quantitation of 29 specific polychlorinated biphenyl (PCB) congeners and 15 chlorinated pesticides in human serum. Analyte surrogates PCB 30, PCB 204, 2,2′,4,4′,5,5′-hexa-bromo-biphenyl, perthane, α-hexachiorocyclohexane, and dichlorobenzophenone were added to each sample. The serum was extracted with an organic solvent and separated by adsorption chromatography into 3 elution fractions for high-resolution gas chromatographic analysis. Each fraction was analyzed by dual-column capillary chromatography followed by electron capture detection. Two capillary columns, DB-5 and DB-1701, with different polarities were used to increase selectivity for each analyte. Quantitation was performed by selecting 2 sets of calibration standard mixtures and 1,2-di-chloronaphthalene as an internal standard. Mean recoveries ranged from 39 to 126% for selected analytes and from 31 to 88% for surrogates. Detection limits for specific congeners and pesticides are reported. Typical chromatographic profiles of calibration standard mixtures, as well as a human sample, are illustrated. Verification of each analyte is assessed, and results of analyses of selected human samples and quality control criteria used to ensure data validity also are presented.

Multiresidue Determination of Endosulfan and Metabolic Derivatives in Human Adipose Tissue Using Automated Liquid Chromatographic Cleanup and Gas Chromatographic Analysis

“…Humans are exposed to OCs through diet and other sources, especially workplace exposure, and OCs are usually detected in human tissues and fluids. Thus, compounds as [3-HCH, p,p'-DDE, or hexachlorobenzene (HCB) are present in most of serum samples analyzed (11)(12)(13). In addition, individuals employed in intensive greenhouse agriculture in Southern Europe have been shown to be subject to high exposure levels (14,15).…”

Biomonitoring of mercury and persistent organic pollutants in Michigan urban anglers and association with fish consumption

“…Mercury was measured in whole blood by inductively coupled plasma-mass spectrometry (ICP-MS) (Rodushkin et al, 1999; NCEH, 2004). PCBs and DDT/DDE were measured using gas chromatography with electron capture detection (GC-ECD) using an in-house method adapted from previous publications (Burse et al, 1990; Najam et al, 1999). Briefly, lipid separation was performed using Florisil column chromatography with 60–100 mesh pesticide residue grade packing.…”

“…Further fractionation was accomplished by 3% deactivated Silica Gel. All fractions were concentrated to 1.0 mL and analyzed by GC-ECD (Burse et al, 1990; Najam et al, 1999). In accordance with program requirements, the MDHHS laboratory provided documentation of Clinical Laboratory Improvement Amendments (CLIA) certification, participated in appropriate external proficiency testing programs, provided proficiency testing results, and provided standard operating procedures for all analytical methods including detailed quality control and quality assurance procedures.…”

DDE and PCB serum concentration in maternal blood and their adult female offspring

“…Whole blood for the analysis of DDE and PCBs was collected and the serum was stored as described above. DDE and individual PCB congeners were extracted and measured by the Analytical Section Chemistry Laboratory at MDCH using high-resolution gas chromatography with electron capture detection according to modifications of the procedure reported previously (Mullin et al, 1984;Najam et al, 1999). Seventy-three PCB congener peaks were identified using a dual column approach.…”