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建立了气相色谱法测定吉非替尼生产中所使用的10种有机溶剂和1个起始原料N-(3-氯丙基)吗啉的残留量。使用DB-624毛细管色谱柱,采用毛细管直接进样,以N-甲基吡咯烷酮∶氯仿(1∶99)为溶剂,程序升温,测定DMF、DMSO和N-(3-氯丙基)吗啉。上述3种物质的回收率为99.6%~101.8%,RSD均小于2.8%。同样使用DB-624毛细管色谱柱,采用毛细管顶空进样,以1%N-甲基吡咯烷酮水溶液为溶剂,程序升温,测定甲醇、丙酮、异丙醇、二氯甲烷、甲基叔丁醚、正己烷、氯仿和正丁醇。上述8种有机溶剂完全分离,回收率为98.2%~109.6%,RSD均小于4.2%。
Gas chromatography was developed to determine the residual amount of 10 organic solvents and 1 starting material N- (3-chloropropyl) morpholine used in the production of gefitinib. DB-624 capillary column was used for direct injection of captopril and N, N-methylpyrrolidone: chloroform (1:99) as solvent. The temperature was programmed to determine DMF, DMSO and N- (3-chloropropyl) morpholine. The recoveries of these three substances ranged from 99.6% to 101.8% with RSDs less than 2.8%. In the same way, DB-624 capillary column was used for capillary headspace sampling and 1% N-methylpyrrolidone aqueous solution was used as the solvent. The temperature was programmed and methanol, acetone, isopropanol, methylene chloride, methyl tert- N-hexane, chloroform and n-butanol. The above 8 kinds of organic solvents were completely separated, the recoveries were 98.2% ~ 109.6%, RSDs were less than 4.2%.