US EPA

2176823 

Journal Article 

Simplified cleanup procedures for adipose tissue containing polychlorinated biphenyls, DDT, and DDT metabolites 

Smrek, AL; Needham, LL 

1982 

Yes 

Bulletin of Environmental Contamination and Toxicology
ISSN: 0007-4861
EISSN: 1432-0800 

28 

6 

718-722 

English 

6809084 

10.1007/BF01605642 

WOS:A1982NS89800014 

The usual procedure for the analyses of chlorinated pesticides in adipose tissue requires that the fat be separated from the connective tissue and then partitioned by liquid-liquid extraction to remove many endogenous interferants. The solvent phase containing the pesticides is further cleaned up by column chromatography (MILLS et al. 1963). The partitioning step is tedious and time-consuming and can be a source of incomplete recovery of some chlorinated pesticides. An effective but potentially hazardous method, in which concentrated sulfuric acid is used, has also been reported for the cleanup of animal tissues (MURPHY 1972).

Anticipating the need for an analytical micro procedure for determining polychlorinated biphenyls (PCBs), dichlorodiphenyltrichloroethane (DDT) and DDT metabolites in several hundred adipose samples taken by needle biopsy, surgery, or autopsy, we developed an analytical micro procedure that eliminates the need for liquid-liquid partitioning in the cleanup of chlorinated pesticide residues in fat samples. In our procedure, the column chromatography step fulfills the function of both the partitioning and column chromatography steps. For the analysis of DDT and DDT metabolites, a 44% sulfuric acid on silica gel chromatography column is used to remove the bulk of lipids and other oxidizable components from the hexane extract. For the analysis of PCBs, a 10% silver nitrate on silica gel chromatography column is used to retain the lipids, DDT and DDT metabolites. We have reported the use of this column for analyzing serum samples for PCBs (NEEDHAM et al. 1980).