Impurity profiling of ecstacy and amphetamine seizures was accomplished by solid-phase microextraction (SPME) combined with capillary gas chromatography (GC). Samples were dissolved in 0.1 M aqueous acetate buffer (pH 5.0) as the only manual operation and subsequently subjected to SPME-GC. Ecstacy tablets were analyzed by head-space SPME to avoid contamination of SPME fibers with insoluble tablet components, while illicit amphetamine powders were exposed to immersed SPME. A SPME fiber of polydimethylsiloxane- divinylbenzene was found to provide excellent extraction of both polar and non-polar impurities. For both illicit ecstacy and amphetamine, complex impurity profiles were obtained by SPME providing a high information content. For ecstacy, profiles (relative peak areas) were repeatable within 2.2 to 12.6% RSD (n = 6), while similar data on amphetamine varied between 2.0 and 10.9 % RSD (n = 6). No carry-over was observed although each fiber was used for 50 to 100 extractions.