The separation of 2′-AMP，3′-AMP and 5′-AMP were investigated by a nonaqueous capillary electrophoresis（NACE) method.Effects of pH* value，nonaqueous solvent，different category buffer on the separation efficiency were studied.The optimum separation conditions are as follows:running medium:200 mmol?L-1 Tris-H3BO3 containing 50% acetonitrile，pH* value:10.0; applied electric field:25 kV; column temperature:25 ℃; detection wavelength:260 nm，and samples were injected from the cathodal end of the capillary by 50 mbar for 5 s.Under the optimal conditions，there are excellent linearities between peak heights and concentrations of the analytes in the concentration range of 1-100 mg/L.The spiked recoveries ranged from 88% to 106% with RSDs less than 4%.The method was applied in the determination of adenosine samples with satisfactory results.