顶空气相色谱法测定甲钴胺原料药的7种溶剂残留

Determination of 7 residual solvents in mecobalamin by headspace gas chromatography

目的建立能同时测定甲钴胺原料药中7种残留溶剂的顶空气相色谱法。方法采用Agilent DB-WAX石英毛细管色谱柱(30 m×0.32 mm,0.5μm)程序升温,进样口温度:220℃;氢火焰离子化检测器(FID)温度:250℃;顶空平衡温度:80℃;平衡时间:30 min。结果7种残留溶剂完全分离,精密度RSD值在0.30%~2.68%范围内,r值均大于0.9991,平均回收率在84.07%~99.56%范围内。结论所用方法操作简单、结果准确,可用于测定甲钴胺中的残留溶剂。

Objective To establish a headspace gas chromatography method for the determination of 7 residual solvents in mecoba-lamin.Methods The residual solvents in mecobalamin were separated and detected by Agilent DB-WAX capillary column(30 m×0.32 mm,0.5μm).The column temperature was programmed.The inlet temperature was 220℃and flame ionization detector(FID)temperature was 250℃.The temperature of balance for the sample was 80℃and the time was 30 min.Results The 7 residual solvents were completely separated.The precision RSDs were 0.30%-2.68%,r values were over 0.9991.The average recoveries were 84.07%-99.56%.Conclusion The method developed was easy and accurate,and it is suitable for the analysis of organic solvent residues in mecobalamin.