HPLC analysis of Atorvastatin Calcium showed an unknown compound peak, the sample was also analyzed by LCMS and the corresponding peak was identified at m/z 854.06. The pure compound was prepared individually and characterized. The compound structure was assigned as tert-butyl 2-((4R,6R)-6-(2-(2-((4R,6R)-6-(2-[2-(4-fluorophenyl)-5-isopropyl-3-phenyl-4-phenylcarbamoyl-pyrrol-1-yl]-ethyl)-2,2-dimethyl-1,3-dioxan-4- yl)acetamido)ethyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetate.