Here we describe a simple, stable, and specific gas chromatography-mass spectrometry (GC-MS) method for the determination of nevirapine in plasma. After precipitation of proteins, the non-nucleoside reverse transcriptase inhibitor nevirapine was extracted with dichloromethane. For the determination and quantification of nevirapine, 1 microL of the organic layer was injected onto the GC-MS system. Linear calibration curves were obtained with BIRH 0414BS as internal standard in a range from 0.01 to 15 microg/mL. Intra- and inter-day accuracy and precision of this method were good with an accuracy between 96-109% and a precision between 2-8% across the therapeutic range of nevirapine. GC-MS proved to be a valid alternative to high-performance liquid chromatography and liquid chromatography-MS.