顶空气相色谱法测定西达本胺原料药中有机溶剂残留量

Determination of Residual Organic Solvents in Chidamide Bulk Drug by Headspace GC

目的建立西达本胺原料药中4种残留溶剂的气相测定方法。方法采用顶空毛细管气相色谱法测定,SPB-1毛细管气相色谱柱(30m×0.32mm×0.5μm),进样口温度:180℃,进样量0.1mL,分流比1∶1;柱温:40℃,保持4min,12℃/min升温至100℃,再以40℃/min升温至220℃,保持4min;检测器为FID,温度:250℃;载气:N2,恒流:2mL·min-1;溶剂为N,N-二甲基乙酰胺。结果各残留溶剂均可以达到基线分离。测得甲醇、二氯甲烷和四氢呋喃线性关系良好。甲醇、二氯甲烷和四氢呋喃的平均回收率分别为98.23%(n=6)、97.87%(n=6)、99.15%(n=69)。结论该法操作简便,重现性好,结果准确可靠,可以用于西达本胺中残留溶剂的测定。

OBJECTIVE To establish a method to determine residual solvents in Chidamide bulk drug.METHODS The headspace GC was carried out with SPB-1 capillary column(30m×0.32mm×0.5μm).The inlet temperature was 180℃.The injection volume was 0.1mL and separation ratio was 1∶1.The column temperature was programmed:the initial temperature was 40℃,maintained for 4min,raised to 100℃with a rate of 12℃/min,and raised to 220℃with a rate of 40℃/min,then maintained for another 4min.The detector was FID with the temperature of 250℃.The carrying gas was N2 with the flow rate of 2mL·min^-1.DMA was used as solvent for Chidamide.RESULTS All solvents can be separated completely with good linear relationship.The average recoveries of acetone,acetonitrile,methylbenzene were 98.23%(n=9),97.87%(n=9),99.15%(n=9)respectively.CONCLUSION This method is simple,reproducible and accurate enough for determination of residual solvents in Chidamide bulk drug.