气相色谱法测定吡非尼酮原料药中的残留溶剂  

Determination of Residual Solvent in Pirfenidone by GC

作　　者：弓全胜[1] 周铁玲 李慧义[1] 田颂九[1] 冯芳[3] 

机构地区：[1]中国药品生物制品检定所,北京100050 [2]上海睿星基因技术有限公司 [3]中国药科大学

出　　处：《中国药事》2006年第9期529-531,共3页Chinese Pharmaceutical Affairs

摘　　要：建立吡非尼酮原料药中有机溶剂残留量的分离测定方法。采用气相色谱法，DB-624石英毛细管柱，氢火焰离子化检测器（FID），程序升温，检测器温度为300℃。3种有机溶剂完全分离，在所考察的浓度范围内具有良好的线性，线性范围：乙酸乙酯49．7～4968．8gg·ml^-1，r=1；N，N-二甲基甲酰胺8．6～858．6μg·ml^-1，r=0．9999；溴苯3．8～383．6gg·ml^-1，r=0．9999。平均回收率为100．8％～102．0%，检测限为0．38～0．86μg·ml^-1。经方法学验证，该方法灵敏度、准确度均达到有机溶剂残留的检测要求，可用于吡非尼酮原料中3种有机溶剂的同时检测。A GC method for separating and determining residual organic solvent in pirfenidone was established. A DB-624 quartz capillary column and a FID were used. The FID was 300℃ by programmed temperature. The three solvents were completely separated and the linear range was 49.7～4968.8 μg·ml^-1 （r=l）, 8.6～858.6 μg·ml^-1 （r=0.9999） and 3.8～383.6μg·ml^-1（r=0.9999） for ethyl acetate, N, N- dimethylformamide and bromobenzene respectively. The average recovery rate was 100.8% ～102.0% and the detection limit was 0. 38～0.86μg·ml^-1. It was validated that the method was sensitive and accurate for residual organic solvents determination in Pirfenidone.

关 键 词：气相色谱法 有机溶剂残留量 吡非尼酮 

分 类 号：R927[医药卫生—药学]