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Simultaneous anodic adsorptive stripping voltammetry was applied for selective and sensitive electrochemical determination of the flavones luteolin (LU) and the basic flavone core 3‐hydroxyflavone (3HF) using a renewable pencil graphite electrode (PGE). The increased separation of the anodic peak potential of LU and 3HF on a PGE surface together with the increased sensitivity renders their simultaneous determination feasible by square wave anodic adsorptive stripping voltammetry (SWAASV). The electrochemical parameters such as surface concentration (Γ), electron transfer coefficient (α), and the standard rate constant (ks) of both LU and 3HF at a PGE were calculated. For simultaneous detection of both compounds by synchronous change of the concentration of LU and 3HF, the detection limits were 1.34 nM and 5.15 nM, respectively. The proposed procedure was successfully applied for the simultaneous detection of LU and 3HF in human serum and urine samples with satisfactory results. [ABSTRACT FROM AUTHOR]