A method using headspace solid-phase microextraction (HS-SPME) then gas chromatography-mass spectrometry with selected ion monitoring (GC-MS, SIM) has been developed for determination of trace amounts of the fungicides pyrimethanil and kresoxim-methyl in soil and humic materials. Both fungicides were extracted on to a fused-silica fibre coated with 85 microm polyacrylate (PA). Response-surface methodology was used to optimise the experimental conditions. For soil samples the linear dynamic range of application was 0.004-1.000 microg g(-1) for pyrimethanil and 0.013-1.000 microg g(-1) for kresoxim-methyl. The detection limits were 0.001 microg g(-1) and 0.004 microg g(-1) for pyrimethanil and kresoxim-methyl, respectively. HP-SPME-GC-MS analysis was highly reproducible-relative standard deviations (RSD) were between 6.7 and 12.2%. The method was validated by analysis of spiked matrix samples and used to investigate the presence of pyrimethanil and kresoxim-methyl above the detection limits in soil and humic materials.