A new quantitative determination method of proteins using beryllon ?by voltammetric technique was developed in this paper. In pH 3.5 Britton-Robinson (B-R) buffer solution, beryllon ?can bind with human serum albumin (HSA) to form an electro-inactive supermolecular complex. Beryllon ?has a well-defined voltammetric reduction peak at 0.38 V (vs. SCE) and the addition of protein in this solution can cause the decrease of the reductive peak current. Based on the decrease of the reduction peak current, a new electrochemical method for the determination of HSA was established with linear range of 1.0~40.0 mg/L and the detection limit of 1.0 mg/L. This method is further applied to the determination of real sample of healthy human serum. A new quantitative determination method of proteins using beryllon® by voltammetric technique was developed in this paper. In pH 3.5 Britton-Robinson (BR) buffer solution, beryllon® can bind with human serum albumin (HSA) to form an electro-inactive supermolecular complex Beryllon? Has a well-defined voltammetric reduction peak at 0.38 V (vs. SCE) and the addition of protein in this solution can cause the decrease of the reductive peak current. Based on the decrease of the reduction peak current, a new electrochemical method for the determination of HSA was established with a linear range of 1.0 to 40.0 mg / L and the detection limit of 1.0 mg / L. This method is further applied to the determination of real sample of healthy human serum.