Determination of the Potential Genotoxic Impurities in Oxiracetam Raw Material by GC-MS / 中国药师

ABSTRACT

Objective:To establish a method for the determination of the potential genotoxic impurities [ methyl chloroacetate and ( R, S) 4-ethyl chloro-3-hydroxybutyrate ] in oxiracetam raw material .Methods:GC-MS was conducted , and the potential genotoxic impurities were extracted by ethyl acetate .The column was a VF-1701 ms capillary column (30 m ×0.25 mm, 0.25 μm) with pro-grammed temperature and the inlet temperature was 220 ℃.The column flow was 1.0 ml· min-1 and the purge flow was 5.0 ml· min-1 .The split injection was used and the split ratio was 51 .The carrier gas was high purity helium and the detector was a mass spectrometer detector .The ion source temperature was 230℃and the interface temperature was 230 ℃.The delay time of solvent was 4 min and the ionization mode was electron impact .The scanning ( detection ) method was selective ion monitoring , the electron energy was 70 eV, and the injection volume was 1.0 μl.Results:The separation between the impurities met the requirements .The concen-tration linear range was 50-400 ng· ml-1 (r≥0.9995).The recoveries were 89.7％-96.3％ (RSD=2.3％, n=9) and 91.0％-105.3％(RSD=4.4％, n=9), respectively.Conclusion:The method is simple, accurate, sensitive and rapid, and can be used for the determination of two potential genotoxic impurities in oxiracetam raw material .