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目的采用直接进样气相色谱法测定比沙可原料药中N,N-二甲基甲酰胺(DMF)的残留量。方法采用DB-624毛细管色谱柱(60.0 m×0.53 mm,3.0μm),进样口温度230℃,氢火焰离子化检测器温度250℃,程序升温:初始温度90℃,保持10 min,以40℃·min~(-1)速率升温至190℃,载气为氮气,流速3.0 m L·min~(-1);直接进样,分流比10∶1,进样体积1.0μL,以甲醇为溶解介质。结果 DMF与溶剂峰的分离度良好,其浓度与峰面积呈良好的线性关系,精密度良好,DMF的RSD=1.5%(n=6),回收率为99.8%~100.9%。结论所用方法适用于比沙可啶原料药中DMF残留溶剂的测定。
OBJECTIVE To determine the residual amount of N, N-dimethylformamide (DMF) in bixacola starting material by direct injection gas chromatography. Methods The temperature of the inlet was 230 ℃ and the temperature of the flame ionization detector was 250 ℃. The programmed temperature was set as follows: the initial temperature was 90 ℃, kept at 10 ℃ for 40 min, The flow rate was 3.0 m L · min -1. The direct injection and the split ratio were 10: 1. The injection volume was 1.0 μL. The methanol was Dissolve media. Results The separation of DMF and solvent peak was good. The linearity of the peak was positively correlated with the precision of DMF. The RSD of DMF was 1.5% (n = 6) and the recovery was 99.8% -100.9%. Conclusion The method is suitable for the determination of DMF residual solvents in bisacodyl drug.