A method is presented for the routine analysis of amphetamine, methamphetamine, and related compounds in urine with gas chromatography coupled with mass spectrometry operated in the selective ion monitoring mode. The analytes are isolated by liquid-liquid extraction and are derivatized with trifluoroacetic anhydride. 3,4-Methylenedioxy-methamphetamine-D(5) is employed as the internal standard. Standard solutions are prepared using spiked urine samples, which are subjected to all phases of sample preparation. Disposable deactivated glass containers are employed throughout the process.