建立了气相色谱法测定吡仑帕奈原料药中的5种残留溶剂四氢呋喃、乙醇、乙腈、吡啶、N,N-二甲基甲酰胺及有关物质1,3-丙二醇.使用DB-WAX型色谱柱,采用直接进样,以二甲基亚砜为空白溶剂,程序升温.结果显示,上述5种有机溶剂及1,3-丙二醇回收率均在97.65%~112.88%,RSD均小于5.0%.在线性试验中,各分析物的峰面积与其质量浓度线性关系良好,相关系数均大于0.998.
A GC method was established for the determination of the five residual organic solvents(tetrahydrofuran,ethanol,acetonitrile,pyridine,N,N-dimethylformamide)and a related substance(1,3-propanediol)in perampanel raw materials.Tetrahydrofuran,ethanol,acetonitrile,pyridine,N,N-dimethylformamide and 1,3-propanediol were quantitatively determined by direct sampling on DB-WAX column,with DMSO as the solvent and temperature programmed control.The above five organic solvents and 1,3-propanediol were completely separated.Their average recoveries were 97.65%-112.88%,with RSDs less than 5.0%.In the linearity test,good linear relationships between peak areas and mass concentrations of the analytes were achieved,and all the correlation coefficients were more than 0.998.