The potential of immunoaffinity-based solid-phase extraction (IASPE) coupled on-line to gas chromatography (GC) for the determination of micropollutants was studied with emphasis on the interfacing of the immunoaffinity-based SPE and GC parts of the system. The cartridge containing the immobilized antibodies was coupled to the gas chromatograph via a reversed-phase cartridge (copolymer sorbent). After trace enrichment of the analytes on the immunoaffinity cartridge, they were desorbed and recollected on the reversed-phase cartridge by means of an acidic buffer. After clean-up and drying with nitrogen, desorption and transfer to the GC was done with ethyl acetate via an on-column interface in the partially concurrent solvent evaporation mode. The antibodies used in the immunoaffinity cartridge were raised against atrazine; several s-triazines were used as test compounds. Triazines that were structurally similar to atrazine, showed quantitative recovery. As an application, immunoaffinity SPE-GC was used for the analysis of river and waste water and orange juice. The selectivity of the system was such that non-selective flame ionization detection (FID) could be used to detect the analytes of interest in these complex matrices. The detection limits for 10-ml water samples were 15-25 ng/l for FID and about 1.5 ng/l for the nitrogen-phosphorus detection. Copyright (C) 1999 Elsevier Science B.V.