Multi-residue method for the determination of chlorinated phenol metabolites in urine.
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Biomedical subjects
Publications and source records attributed to R F Moseman.
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The pollution of the environment with Kepone (decachlorooctahydro-1,3,4-metheno-2H-cyclobuta[cd]pentalen-2-one) by an industrial manufacturer of the pesticide resulted in the contamination of several terrestrial media, including biological life, near the entry of the insecticide into the ecosystem. The substrata investigated and for which residue methodology was developed included river sediment, soil, water, shellfish, and finfish. Rigorous extraction techniques utilizing the Soxhlet apparatus and the Polytron tissue homogenizer were required for complete removal of Kepone from the samples. Finfish tissue was the most difficult to analyze. For this type of substratum, a preliminary cleanup by gel permeation chromatography was required to remove most of the lipid material followed by a micro Florisil column elution to eliminate polychlorinated biphenyls (PCB'S). Cleanup of shellfish and other environmental samples was accomplished with a micro Florisil column only. Electron capture gas chromatography was used to analyze the sample extracts. Recoveries of Kepone from fortified samples averaged 84% or greater.
Simplified methodology is presented for the micro determination of polychlorinated biphenyls (PCBs) in biological samples, by conversion to the decachlorobiphenyl (DCB) derivative. Beef adipose tissue and human milk extracts were fortified with PCB standards at 0.1--5.0 ppm, and perchlorinated with antimony pentachloride (SbCl5). Several Aroclors representing various degrees of chlorine content were investigated to assess the efficiency of conversion to DCB. Samples were cleaned up on a Florisil mini column and the PCBs were quantitated by electron capture GLC. Several chlorinated pesticides which were subjected to the perchlorination procedure did not interfere. As little as 0.1 ppm PCBs in 500 mg tissue extract can be recovered at 79-99%. The background DCB content of several brands of SbCl5 was determined. The levels of PCBs in human milk obtained by the perchlorination technique are compared with data acquired by electron capture gas-liquid chromatography in which the individual chlorobiphenyls in the sample are measured.
Several mono- and dihydroxy metabolites of di-, tri, and tetrachlorobiphenyl have been identified in the urine of rats fed prolonged diets of Aroclor 1016 or Aroclor 1242. Combined gas chromatography-mass spectrometry was used for characterization of the metabolic products.
The described procedure can be utilized for rapid, simple quantitation and confirmation of hexachlorobenzene in fatty tissue at levels as low as 5 ppb without the use of sophisticated and expensive equipment. Interferences can be circumvented in many instances without additional separation by selection and preparation of the appropriate derivative.
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The analyses of four organophosphorus pesticide poisoning cases, three of which resulted in death, are reported. The case histories of the subjects, along with the analysis of tissues, urine, and blood for the levels of pesticides and metabolites are given. The pesticides involved include dicrotophos, chlorpyrifos, malathion, and parathion. The methods of analysis were adapted from previously published methods that provide a very rapid means of identification of organophosphorus pesticides in the tissues or in the blood of poisoned patients.