Separation of lipophilic substances in environmental samples with special reference to toxaphene

A microcolumn of alumina, activated at 250 degrees C over night and deactivated with 2% water in an oven at 150 degrees C, has shown better separation characteristics than similar ones, deactivated at room temperature, for a great number of organochlorine compounds, particularly with respect to multicomponent toxaphene and PCB. The microcolumn is a simple disposable Pasteur pipette. Three fractions are collected: one with PCB and DDE, one with toxaphene components having similar lipophilicity to DDT and the third, toxaphene components similar to DDD in lipophilicity. Two such toxaphene fractions give a better GLC-pattern than only one fraction. DDD and DDT, which interfere with the analysis of toxaphene can be eliminated, after their GLC analysis, from the "Toxaphene fractions" by nitration followed by reduction of the nitro compounds formed to their corresponding amines. Performance of the column using environmental samples showed that it is a useful tool in routine pesticide residue analysis, especially when toxaphene is present.