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
| Autor: | Larry L. Needham, Margaret P Korver, Cynthia C Williams, Virlyn W. Burse, Allah R Najam |
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| Rok vydání: | 1999 |
| Předmět: | |
| Zdroj: | Journal of AOAC INTERNATIONAL. 82:177-185 |
| ISSN: | 1944-7922 1060-3271 |
| DOI: | 10.1093/jaoac/82.1.177 |
| Popis: | 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. |
| Databáze: | OpenAIRE |
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