顶空毛细管气相色谱法测定二氟尼柳原料药中的残留溶剂

Head-Space Sampling Capillary GC for Determing Residual Solvents in Raw Material Drug of Diflunisal

采用Agilent DB-624毛细管色谱柱(25 m×0.53 mm×3.0μm),FID检测器,N,N-二甲基甲酰胺为溶剂,进行了顶空毛细管气相色谱法同时测定二氟尼柳原料药中二氯甲烷、苯及甲苯等3种残留溶剂的分析方法试验。结果表明,3种残留溶剂在各自的含量范围内呈良好的线性关系(相关系数0.994 5～0.997 5),检测限分别为0.012 8、0.044 8、0.189 mg/L,平均添加回收率为90.6%～97.9%。所建方法简单、灵敏、可靠,适用于二氟尼柳原料药中残留溶剂的分析检测。

A capillary GC method with head-space sampling was established for determing residual solvents such as dichloromethane,benzene and methylbenzene in raw material drug of Diflunisal.Agilent DB-624 capillary column(25 m×0.53 mm×3.0 μm) was used,FID as detector and DMF as the solvent.The result showed that linear responses were obtained for the 3 residual solvents in their respective concentration ranges(R=0.994 5~0.997 5,n=5).The average recoveries of three concentration levels were 90.6%~97.9%.The developed method simple,sensitive and accurate for the residual solvent analysis in raw material drug of Diflunisal.