Sixteen novel conjugates of madecassic acid and silybin have been synthesized through esterification or using amino acids as linkers. The formation of esters at positions 3 or 7 could be controlled depending on the reaction conditions. The new conjugates were evaluated for their cytotoxicity on the HepG2 liver cancer cell lines HepG2. Nine compounds showed higher cytotoxic activity than that of silybin and five compounds exhibited greater cytotoxic activity than madecassic acid itself. Among dosage, but also giving biological properties which are enhanced or distinct from the two molecules individually.