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

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.