Psychedelic phenethylamines are an emerging class of designer drugs capable of producing a complex array of sought after adrenergic and hallucinogenic effects. Toxicological detection poses a number of challenges to laboratories. The purpose of this study was to develop a procedure for the detection of psychedelic amphetamines using techniques that are widely accepted in forensic toxicology laboratories. In all, 10 target analytes were selected: 2,5-dimethoxy-4-bromophenethylamine (2C-B), 2,5-dimethoxyphenethylamine (2C-H), 2,5-dimethoxy-4iodophenethylamine (2C-I), 2,5-dimethoxy-4ethylthiophenethylamine (2C-T-2), 2,5-dimethoxy-4-(n)propylthiophenethylamine (2C-T-7), 4-methylthioamphetamine (4-MTA), 2,5-dimethoxy-4-bromoamphetamine (DOB), 2,5-dimethoxy-4-ethylamphetamine (DOET), 2,5-dimethoxy4-iodoamphetamine (DOI), and 2,5-dimethoxy-4methylamphetamine (DOM). Target drugs in urine were analyzed by gas chromatography in selected ion monitoring mode after mixed-mode solid-phase extraction. Limits of detection for all analytes were 2-10 ng/mL, and limits of quantitation were 10 ng/mL or less. Precision evaluated at 50 and 500 ng/mL yielded CVs of 0.4-7.9% and accuracy in the range 91-116%. Calibration curves were linear to 1500 ng/mL using mescaline-d₉ as the internal standard. No carryover was evident at 5000 ng/mL (the highest concentration tested) and no interferences were observed from the presence of other structurally related compounds or endogenous bases.