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 6M/40 degrees 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 ((1)H NMR, (13)C NMR, DEPT, MS and IR), formation and mechanism has been discussed in detail.
Bharathi
Ch
Ch
A.P.L. Research Centre, 313 Bachupally, Hyderabad 500072, India.
Chary
D Krishnama
DK
Kumar
M Saravana
MS
Shankar
Rama
R
Handa
V K
VK
Dandala
Ramesh
R
Naidu
A
A
D014150:Antipsychotic Agents / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D004340:Drug Contamination; D004355:Drug Stability; D006358:Hot Temperature; D007555:Isoxazoles / Q000737:chemistry* / Q000302:isolation & purification; D008027:Light; D009682:Magnetic Resonance Spectroscopy / Q000379:methods; D013058:Mass Spectrometry / Q000379:methods; D008956:Models, Chemical; D015394:Molecular Structure; D018967:Risperidone / Q000031:analogs & derivatives* / Q000737:chemistry* / Q000302:isolation & purification; D013607:Tablets
C528263:3-(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; D014150:Antipsychotic Agents; D007555:Isoxazoles; D013607:Tablets; D018967:Risperidone