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Original Articles

Enrichment of Trace Chlorinated Species in a Complex Matrix of Fatty Acids Using HPLC in Conjunction with Gas Chromatography‐Halogen Specific Detection

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Pages 1809-1826 | Received 20 Dec 2002, Accepted 21 Jan 2003, Published online: 06 Feb 2007
 

Abstract

Due to the similarity in chemical and physicochemical properties between analytes (chlorinated fatty acids) and matrix compounds (nonchlorinated fatty acids), conventional cleanup procedures were not successful in analysis of chlorinated fatty acids in extracts of freshwater fish. A new approach was devised of utilizing reversed‐phase high performance liquid chromatography (HPLC) for its high separation power, and the halogen specific detector (XSD) for its high selectivity for organochlorine. The bulk of nonchlorinated matrix was removed by HPLC fractionation, and target chlorinated analytes were selectively enriched. The enrichment effect was assessed by a universal detector, a flame ionization detector (FID). Methyl esters of chlorinated fatty acids were completely nondetectable prior to HPLC fractionation, but were present as moderate or small, yet discernible, peaks after the HPLC enrichment. This enrichment method is efficient with good selectivity, reproducibility, and predictability.

Acknowledgments

This work was part of the consortium “Using Chemistry and Biology to Improve Bleaching Effluent Quality” at the University of Toronto Pulp & Paper Centre, funded by Alberta Pacific Forest Industries Inc., Aracruz Cellulose SA, Avenor Inc. (now Bowater Pulp and Paper Canada Inc.), Boise Cascade Corp., Georgia‐Pacific Corp., International Paper, Irving Forest Services Ltd., Japan Carlit Co. Ltd., Nippon Paper Industries Co. Ltd., Ontario Ministry of Environment & Energy, Potlatch Corp., Sterling Pulp Chemicals Ltd., Tembec Inc., and Weyerhaeuser Co. We thank Dr. Mark Servos and John Toito for assistance in securing fish samples, and Ivy D'sa, Sean Backus and Dr. Mohan Kohli for laboratory support in GC‐XSD operation.

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