顶空气相色谱法测定吡仑帕奈中5种有机溶剂

Determination of five organic solvents in perampanel by headspace gas chromatography

建立测定吡仑帕奈原料药中甲醇、乙酸乙酯、四氢呋喃、吡啶和N,N-二甲基甲酰胺5种有机溶剂残留量的顶空气相色谱法。采用Agilent DB-624毛细管色谱柱(30 m×0.32 mm,1.8μm)分离,程序升温,进样口温度为250℃,氢火焰离子化检测器温度为250℃,顶空进样平衡温度为100℃,平衡时间为20 min。在以上色谱条件下5种溶剂完全分离,在各自范围内线性关系良好(r≥0.9994),检出限为0.14~0.92μg/mL,平均加标回收率为97.14%~103.62%,测定结果的相对标准偏差为1.28%~3.33%(n=9)。该方法操作简单、灵敏准确,可用于吡仑帕奈中5种残留溶剂的检测与分析。

A headspace gas chromatography method was established to determine 5 residual solvents of methanol,ethyl acetate,tetrahydrofuran,pyridine and N,N-dimethylformamide in perampanel.The residual solvents in perampanel were separated by Agilent DB-624 capillary column(30 m×0.32 mm,1.8μm).The column temperature was programmed.The inlet temperature was 250℃,the flame ionization detector(FID)temperature was 250℃.The temperature of balance for the sample was 100℃and the balance time was 20 min.Under the above test conditions,5 residual solvents were completely separated.There were good linear relationships with the correlation coefficients of more than 0.9994.The detection limits were 0.14-0.92μg/mL.The average recoveries were 97.14%-103.62%,and the relative standard deviations were 1.28%-3.33%(n=9).The method developed is easy,sensitive and accurate,and it is suitable for the analysis of 5 solvent residues in perampanel.