吉非替尼中残留溶剂的GC法测定

Determination of Residual Organic Solvents in Gefitinib by GC

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%。

A GC method was established for the determination of ten residual organic solvents and a starting material N- （3-chloropropyl） morpholine in gefitinib. DMF, DMSO and N- （3-chloropropyl） morpholine were quantitatively determined by direct sampling gas chromatography （D-GC） on a DB-624 column, with 1-methyl-2- pyrrolidinone ： chloroform （1 ： 99） as the solvent and temperature programmed control. Their average recoveries were 99.6% - 101.8%, with RSDs less than 2.8%. Methanol, acetone, isopropanol, dichloromethane, tert-butyl methyl ether, n-hexane, chloroform and n-butanol were quantitatively determined by headspace gas chromatography （HS-GC） on a DB-624 column, with 1% 1-methyl-2-pyrrolidinone aqueous solution as the solvent and temperature programmed control. The above eight organic solvents were completely separated. Their average recoveries were 98.2 % - 109.6 %, with RSDs less than 4.2%.