In this paper, an atomic absorption spectrometric method has been established to determine adrenaline using Cu(II) as probe reagent. In the presence of SCN−, it has been demonstrated that Cu(II) is reduced to Cu(I) by adrenaline at pH 6.0, and the in situ formed Cu(I) reacts with SCN- to form the white emulsion of CuSCN. According to the amount of residual Cu(II) which is measured by atomic absorption spectrometry, the amount of adrenaline can be determined indirectly. Beer's law is obeyed in the range of adrenaline concentration of 0.080-6.00 mg mL-1, and the linear regression equation is A = 0.20342 - 0.02756C (μg mL−1) with a correlation coefficient of 0.9998. The detection limit is 0.033 μg mL−1 and R.S.D. is 0.56%. This method has been successfully applied to determine adrenaline in pharmaceutical and serum samples with satisfactory results.