(Ti0.5V0.5)3AlC2 is prepared via ball-milling Ti, V, Al, and C precursor powders with mole ratio of 1.5 : 1.5 :1.1 : 1.9 followed by sintering the obtained fine powder at 1400°C for 20 min under argon atmosphere. The morphology and structure of products are characterized by using XRD and SEM techniques. Then Al is chemically etched from synthesized (Ti0.5V0.5)3AlC2 by immersing in 40% HF solution at room temperature for 20 h. The resulting suspension is centrifuged to separate the powder and washed severely with distilled water. Resulting (Ti0.5V0.5)3C2 is used as a new modifier for preparation of carbon paste electrode. Modified electrode based on (Ti0.5V0.5)3C2 shows a good performance for measurement of propranolol concentration in pharmaceutical formulation. The detection limit and the relative standard deviation for n = 5 are 0.16 μmol/L and 4%, respectively.