气相色谱法测定吡非尼酮中残留溶剂含量

目的建立了吡非尼酮中6种有机溶剂残留量的分离测定方法。方法采用溶液直接进样气相色谱法,色谱柱为HP-INNOWAX毛细管柱(30 m×0.53 mm×2.65 m),载气为氮气,以N,N-二甲基甲酰胺为溶剂,测定了吡非尼酮原料药中异丙醚、丙酮、二氯甲烷、乙腈、二氧六环与吡啶的残留量。结果 6种有机溶剂完全分离,在所考察的浓度范围内线性关系良好,其中异丙醚、丙酮、二氯甲烷、乙腈、二氧六环与吡啶的线性范围分别为10.16~1 016μg.mL-1(r=0.999 99),9.92~992μg.mL-1(r=0.999 99),1.272~127.2μg.mL-1(r=0.999 8),0.848~84.8μg.mL-1(r=0.999 8),0.785~78.5μg.mL-1(r=0.999 9),0.416~41.6μg.mL-1(r=0.999 9)。各残留溶剂的精密度试验RSD均小于5%,平均回收率在96.22%~99.97%之间。结论本实验所建立的方法简便、灵敏、准确,可用于吡非尼酮中有机溶剂残留量的测定。

Determination of residual solvents in Pirfenidone by GC

Objective To establish a GC method for the determination of six residual organic solvents in Pirfenidone.Methods The residual organic solvents including isopropyl ether,acetone,dichloromethane,acetonitrile,1,4-dioxane and pyridine were determined by Capillary GC with HP-INNOWAX（30 m×0.53 mm×2.65 m）column.N,N-DMF was solvent,N2 was the carrier gas.Results Six residual organic solvents were completely separated.The linear ranges of isopropyl ether,acetone,dichloromethane,acetonitrile,1,4-dioxane and pyridine were 10.16～1 016 μg·mL-1（r=0.999 99）,9.92～992 μg·mL-1（r=0.999 99）,1.272～127.2 μg·mL-1（r=0.999 8）,0.848～84.8 μg·mL-1（r=0.999 8）,0.785～78.5 μg·mL-1（r=0.999 9）,0.416～41.6 μg·mL-1（r=0.999 9）.The RSDs of precision of residual organic solvents were all less than 5%,the average recovery of the preparation were between 96.22%～99.97%.Conclusion The method was simple,sensitive,accurate and can be used for the determination of residual organic solvents in Pirfenidone.