Abstract: A simple,sensitive and rapid liquid chromatographic-electro-spray ionization tandem mass spectrometric method was developed for the quantification of nebivolol in human plasma.Amlodipine was used as the internal standard(IS).Separation was performed using a Shimadzu C₁₈column (150 mm×2.0 mm,4.6μm) maintained at 35℃ and the mobile phase consisting of a mixture of acetonitrile and water (containing 0.05% formic acid) (45∶55) was delivered at a flow rate of 0.2 mL/min;The analytes were analyzed by electro-spray ionization (ESI) in the selected reaction monitoring mode.The precursor to product ion transitions ofm/z 406.2-151.0 and m/z 409.0-238.2 were used to measure nebivolol and the IS,respectively.The linearity ranged from 0.025 to 25 ng/mL( r = 0.998 6);and the limit of detection of nebivolol in human plasma was 0.008 ng/mL.The recovery,intra- and inter-assay precisions met the requirements of bioanalytical method.Thet_1/2,AUC_0-t,c_max,MRT of nebivolol in healthy volunteers were (14.4±5.5)h,(7.35±2.48) ng?h/mL,(1.05±0.35) ng/mL,and (16.5±5.3)h for a single oral dose of 5 mg nebivolol,respectively.The method is selective and suitable for the quantification of nebivolol in human plasma.