Determination of Residues of Genotoxic Impurity Pivaloyl Chloride in Cefalexin API by HS-GC-MS
Objective:To establish a specific HS-GC-MS method to determination of residues of genotoxic impurity pivaloyl chloride in Cefalexin API.Methods:The separation was performed on a HP-1MS UI capillary column(30 m×0.25 mm,0.5 μm)in a temperature rising program.The carrier gas was helium with flow rate of 1 mL·min-1.The inlet temperature was 200℃,the headspace equilibrium temperature was 70℃,the quantitative ring temperature was 80℃,and the headspace transmission line temperature was 90℃.The sample was ionized by electron ionization.The ion source temperature was 230℃,the quadrupole temperature was 150℃,and the MSD transmission line temperature was 250℃.Detection were performed by mass spectrometry in selective ion monitoring mode with m/z 57.1 for ethyl pivalate.The genotoxic impurity pivaloyl chloride was detected in 4 batches of Cefalexin API following based on the conditions.Results Ethyl pivalate and adjacent chromatographic peaks were separated well and showed good linearity at 50.170 ng·mL-1～501.695 ng·mL-1(r=0.995).The limits of detection and quantification was 12.473 ng·mL-1 and 24.945 ng·mL-1,respectively.The average recovery was 110%,and the RSD was 6.0%(n=9).Conclusion:The method is sensitive and specific,which can be used for the quantification of genotoxic impurity of genotoxic impurity pivaloyl chloride in Cefalexin API.
万方数据
维普
