The preparation selected for examination with this technique contained 4-methoxyamphetamine, an hallucinogenic amphetamine that has been encountered frequently in South Australia. The gas chromatograph used was a Hewlett Packard 5890 equipped with a 5972 MSD and electronic pressure programming. For SPME a glass liner of 0.75 mm internal diameter was used in the injector, and a standard split/splitless liner was used for liquid injections. Helium was used as carrier gas at a constant linear flow rate of 62 cm/second for SPME and 55 cm/second for liquid injection; the column was a 15 m x 0.257 mm x 0.25umDB-1 fused silica capillary; for SPME the oven program went from 50 degrees C to 300 degrees C at a rate of 30 degrees C per min.; for liquid injection the oven program started at 90 degrees C and went to 300 degrees C at 45 degrees C per min.; the injector was kept at 290 degrees C for SPME or 300 degrees C for liquid injection. Compounds found in the PMA preparation included 4-methoxyphenol, 4-methoxybenzaldehyde, 4-methoxyphenyl-2-propanone, 4-methoxyphenyl-2-propanol, 4-methoxyphenyl-propene, and (tentatively) 4-methyl-5-(4'-methoxyphenyl) pyrimidine. The presence of these compounds suggests that the active drug was prepared from 4-methoxybenzaldehyde via 4-methoxyphenyl-2-propanone using a Leuckardt reductive amination. In this instance, SPME was found to be a simple, rapid, and nondestructive recovery technique that gave results complementary to those provided by conventional liquid-liquid extraction. There is an indication that SPME might find application in the profiling of illicit drugs. 4 figures, 1 table, and 10 references