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A solid-phase extraction (SPE) method was developed using 8 M urea to desorb and extract organochlorine pesticides (OCs) and polychlorinated biphenyls (PCBs) from avian serum for analysis by capillary gas chromatography with electron capture detection (GC-ECD). The analytes were efficiently extracted from the denatured serum-lipoprotein-analyte complex by one passage through an Oasis (R) hydrophilic-lipophilic-balanced (HLB) SPE cartridge. No further clean-up was necessary, the entire extraction procedure and GC-ECD analysis can be accomplished in less than 3 h. Serum Volumes ranged from 100 mu L to 1 mL with absolute recoveries of 90-101 % for PCBs and 74% to 101 % for the OC pesticides. (c) 2005 Elsevier B.V. All rights reserved.