US EPA

2210814 

Journal Article 

Multicomponent Analysis Method for PCDDs and PCDFs in Biological Samples 

Tarhanen, J; Paasiverta, J; Soikkeli, J 

1986 

Yes 

Chemosphere
ISSN: 0045-6535
EISSN: 1879-1298 

NIOSH/00167624 

15 

9-12 

10.1016/0045-6535(86)90525-4 

https://linkinghub.elsevier.com/retrieve/pii/0045653586905254
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A procedure for cleanup of polychlorinated dibenzo-p-dioxins (PCDD) and polychlorinated dibenzofurans (PCDF) was presented so that accurate analyses of biological samples could be conducted without interference from other materials, such as polychloroaromatic methyl ethers. Prior to any treatment of the sample, 1,2,3,4-tetrachloro-dibenzo-p-dioxin was added to provide an international standard for quantitation. The tissue sample was then mixed with disodium-sulfate and allowed to stand for 48 hours. The dried mixture was then extracted for 6 hours with an organic solvent mixture of petroleum-spirit/acetone/hexane/diethyl-ether. After evaporation, the residue was weighed and then dissolved in hexane. Fat was first removed with silica gel/concentrated sulfuric-acid paste and then by shaking with concentrated sulfuric-acid. The first fraction eluted included polychlorinated hydrocarbons such as polychlorinated biphenyls, DDE, toxaphene, and chlordanes. Planar aromatic ethers were removed in toluene by reverse elution from the carbon column. The sample was next eluted through an activated basic alumina column where PCDDs and PCDFs were collected as the second fraction. The final determination was done by a gas chromatographic system equipped with two quartz capillary columns and two electron capture detectors. Samples studied by this method included fish liver oil, salmon muscles, and pectoral muscles of the white tailed eagle, each of which were found to contain PCDDs and PCDFs.