Organic impurity profiling of seized 3,4-methylenedioxymethamphetamine (MDMA) tablets aims to link tablets to common production sources. Conventionally, organic impurities are extracted from tablets using a liquid-liquid extraction (LLE) procedure prior to analysis by gas chromatography-mass spectrometry (GC-MS). In this research, the development of an alternative microwave-assisted extraction/headspace solid-phase microextraction (MAE/HS-SPME) procedure is described. The optimal procedure used phosphate buffer (1 M, pH 8), with an HS-SPME extraction temperature of 70 degrees C for 40 min, using a divinylbenzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber. Impurities were extracted from seized MDMA exhibits using the MAE/HS-SPME procedure, as well as HS-SPME alone, and a conventional LLE procedure. The HS-SPME procedure was deemed to be the most practical because of the affordability and need for less analyst involvement. Although the LLE was limited in the number of impurities extracted, the procedure is still useful for the extraction of less volatile impurities that are not extracted by HS-SPME. (Published Abstract)