A new method for the determination of furosemide (CAS 54-31-9) in plasma and urine by gas chromatography/mass spectrometry (GC/MS) has been developed. After acidification the samples were extracted by ethyl acetate and methylated by methyl iodide. The chromatography was carried out on a fused-silica capillary column with SE-54 stationary phase. Detection was performed by selected ion monitoring (ions 81 and 372 were monitored for furosemide and ions 363 and 406 for internal standard bumetanide). Limit of quantitation was 10 ng/ml for plasma and 40 ng/ml for urine and the calibration curves were linear up to 100,000 ng/ml.