||Micromethods for Toxic Residue Screening by Negative Chemical Ionization Mass Spectrometry.
Kuehl, Douglas W. ;
Whitaker, Michael J. ;
Dougherty, Ralph C. ;
||Florida State Univ., Tallahassee. Dept. of Chemistry.;Environmental Reseach Lab.-Duluth, MN.
Chemical analysis ;
Chlorine organic compounds ;
Mass spectroscopy ;
Solvent extracts ;
Polychlorinated biphenyls ;
Toxic substances ;
Biological samples ;
Gel permeation chromatography ;
Chemical ionization mass spectroscopy
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Methods were developed for the analysis of polychlorinated chemical residues found in milligram quantities of biological samples. Sample preparation by micro-continuous liquid-liquid extraction steam distillation or by micro gel-permeation chromatography gave sufficiently clean residue extracts for negative chemical ionization analysis. With these techniques, chemicals such as chlorophenols and chlorobiphenyls have been confirmed in human adipose samples as small as 12.5 mg. These methods make it possible to screen less than 1-g samples of biological substrates for contamination with persistant toxic substances at part-per-billion levels.