The presence of impurities that arise either from the process or the starting materials in bulk drugs is potentiallyundesirable. The presence of these impurities beyond the limit may modify the quality, well-being, and efficiencyof drug products; hence, it has to be controlled based on the current regulatory requirements. These impurities maynot be monitored regularly, but for a minimum of three validations, and a few of the commercial batches are tobevalidated to ensure the impurities are neither leached to the final stage of the process nor below the detection limit. To demonstrate the lowest possible detection of dicyclopentadiene in Saxagliptin drug substances, the newreverse- phase HPLC procedure was designed using by Inertsil C18 column with 0.10% aqueous orthophosphoric acidand0.10% orthophosphoric acid in acetonitrile as mobile phases in gradient elution specification. The results indicatethat the method can detect lower levels of dicyclopentadiene in drug substances with good linearity up to 1500ppm. Further, the established process was validated by ICH regulations, and the greenness of the process was establishedby the AGREE statistical tool.