Abstract: In a base solution of HCl-KCl (pH 1.7),sensitive oxidation and reduction peaks of aloin were observed at the potentials of -0.386 V (Epc) and -0.441 V (Epa) respectively as studied by cyclic voltammetry.Linear relationship between values of reduction peak current (ipa) and concentration of aloin was obtained in the range of 1.20×10-6-2.15×10-4mol·L-1,with detection limit (3S/N) of 4.78×10-7mol·L-1.Based on these facts,a cyclic voltammetric method for determination of aloin in aloe was proposed.In addition,the electrochemical behavior of aloin at GCE was also studied.An shown by the experimental results,the redox reaction of aloin at GCE was an irreversible and adsorptive process.