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目的建立吡非尼酮中残留碘苯含量测定的气相色谱法。方法取吡非尼酮加甲醇溶解稀释后测定。色谱条件:色谱柱为PEG-20M弹性石英毛细管柱(30m×0.22mm0.25μm),载气为氮气;程序升温:起始温度50℃,以25℃/min升温至150℃,保持4min;气化室温度220℃,检测器温度250℃;火焰离子化检测器(FID)检测。结果碘苯在2.14~53.5μg/ml范围内线性关系良好,进样精密度(RSD)为1.99%,平均回收率为99.6%,检测限为0.19μg/ml。结论本法灵敏、准确、重现性好,可用于控制吡非尼酮中残留碘苯的量。
Objective To establish a gas chromatographic method for the determination of residual iodobenzene in pirfenidone. Methods Take pirfenidone dissolved in methanol diluted measured. Chromatographic conditions: the column was PEG-20M elastic quartz capillary column (30m × 0.22mm0.25μm), the carrier gas was nitrogen; temperature programmed: initial temperature of 50 ℃, 25 ℃ / min heating to 150 ℃, holding 4min; gas Room temperature 220 ℃, detector temperature 250 ℃; flame ionization detector (FID) detection. Results The linearity of iodobenzene in the range of 2.14-53.5μg / ml was good. The precision of injection (RSD) was 1.99%. The average recovery was 99.6%. The detection limit was 0.19μg / ml. Conclusion This method is sensitive, accurate and reproducible. It can be used to control the amount of residual iodobenzene in pirfenidone.