Rapid semi-micro method for separating non-ortho chlorinated chlorobiphenyls from other chlorobiphenyls

Analyst Pub Date: DOI: 10.1039/AN9952001917

Abstract

A method for separating common non-ortho chlorinated chlorobiphenyls, namely 3,4,4′-tri-, 3,4,4′,5-, 3,3′,4,4′-tetra, 3,3′,4,4′,5-penta-, and 3,3′4,4′,5,5′-hexachlorobiphenyl (IUPAC Nos. 37, 81, 77, 126, and 169) from other chlorobiphenyls in shellfish tissue at pg g–1 wet mass concentrations is described. The method is based on saponification followed by extraction into 2,2,4-trimethylpentane, clean-up by gel-permeation chromatography and sulfuric acid treatment, separation of non-ortho chlorinated chlorobiphenyls from other chlorobiphenyls using a Florisil–carbon column and measurement using capillary GC–low resolution MS with selected ion monitoring to eliminate many interfering materials. Recoveries of chlorobiphenyls (20–5000 pg g–1 wet mass) averaged 84.5 ± 6.5%. The detection limits (3 times the noise level) are 20 pg g–1 wet mass for IUPAC Nos. 37, 77, 81, and 126 and 50 pg g–1 wet mass IUPAC No. 169. The method gave results for non-ortho chlorinated chlorobiphenyl concentrations in lobster digestive gland tissues and Aroclors equivalent to those obtained by a conventional procedure.

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