Identification, isolation and characterization of potential degradation product in risperidone tablets

One unknown impurity (degradation product) present at a level below 0.1% in the initial samples increased to a level of 0.5% in 6 M/40 °C/75% RH stability samples of risperidone tablets was detected by gradient reverse-phase high-performance liquid chromatography (HPLC). This impurity was isolated using reverse-phase preparative liquid chromatography. Based on the spectral data the structure of this impurity is characterized as 3-[2-[4-[6-fluoro-1,3-benzoxazol-2-yl]piperidin-1-yl]ethyl]-2-methyl-6,7,8,9-tetrahydro-4H-pyrido[1,2-a] pyrimidin-4-one. Structural elucidation of this impurity by spectral data (1H NMR, 13C NMR, DEPT, MS and IR), formation and mechanism has been discussed in detail.