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A method for the determination of digoxin in human serum using a liquid ch rom atograp hy/electrosp ray ionization-tandem mass spectrometry (LGESI-MIS/MS) technique is reported. Digoxin and the internal standard, 121,21,22-(2) H-3]digoxin, were extracted from 250 mu l of human serum using a solid phase extraction cartridge (Oasis HLB) and analyzed by LG/ESI-MS/MS in the selected reaction monitoring mode. The intra- and inter-assay reproducibility and accuracy were satisfactory within the quantification range of 0.20-3.20ng/ml. The concentrations of digoxin in the serum samples obtained from digitalized patients (n=19) were in the range of 0.25-2.84 ng/ml, which were compared to those obtained by radioimmunoassay.