气相色谱法测定吡非尼酮中残留溶剂含量  

Determination of residual solvents in Pirfenidone by GC

作　　者：高瑞银[1] 魏福荣[1] 单鸣秋[2] 丁安伟[2] 

机构地区：[1]江苏吉贝尔药业有限公司,江苏镇江212009 [2]南京中医药大学,江苏南京210046

出　　处：《齐鲁药事》2011年第7期383-384,共2页qilu pharmaceutical affairs

摘　　要：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。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.

关 键 词：吡非尼酮 气相色谱法 残留溶剂 

分 类 号：R927.11[医药卫生—药学]