A micro derivation technique for the confirmation of trace quantities of kepone

Moseman, R.F.; Ward, M.K.; Crist, H.L.; Zehr, R.D.

Journal of Agricultural and Food Chemistry 26(4): 965-968


ISSN/ISBN: 0021-8561
PMID: 78935
DOI: 10.1021/jf60218a001
Accession: 068519748

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A rapid and simple procedure was devised for the confirmation of nanogram quantities of Kepone that is sensitive to part per billion levels in environmental and biological samples. Electron-capture gas chromatography of the perchlorinated derivative enabled confirmation often not possible by other techniques such as gas chromatography combined with mass spectrometry. Conversion of Kepone to mirex was accomplished by a high-temperature closed-tube reaction. Mirex that might have been present in the original sample extract was separated from Kepone by a micro Florisil column cleanup step. The absence of mirex in cleaned-up sample extracts was verified during the electron-capture gas chromatographic quantitation for Kepone. The conversion of Kepone to mirex was quantitative, allowing for the estimation of Kepone by a separate technique. Considerable confidence is added to analytical results. Details of the methodology and results are discussed.