顶空气相色谱法测定ET-26盐酸盐中的7种残留溶剂

Determination of the seven kinds of residual solvents in ET-26 hydrochloride by Headspace GC

目的采用顶空气相色谱法测定ET-26盐酸盐中7种有机溶剂[甲醇、乙醇、丙酮、乙酸乙酯、乙二醇甲醚、溴乙基甲醚、二甲基甲酰胺(DMF)]的残留量。方法甲醇、乙醇、丙酮、DMF为一组,乙酸乙酯、乙二醇甲醚、溴乙基甲醚为另一组,分别采用分流/不分流的顶空气相色谱法,选用DB-624毛细管柱(30 m×530μm,3μm)为分析柱,N2为载气,氢火焰离子化检测器(FID)检测,以程序升温方式使各残留溶剂达到完全分离。结果在两种色谱条件下,7种残留溶剂的线性关系、回收率、精密度及灵敏度均达到了要求。结论所用方法灵敏、准确,可用于ET-26盐酸盐中残留溶剂的检查。

OBJECTIVE To determine the seven kinds of residual solvents （methanol, ethanol, acetone, ethyl acetate, 2 - methoxyethanol, bromoethyl methyl ether and DMF） in ET -26 hydrochloride by Headspaee gas chromatographic. METHODS Seven kinds of organic solvents were divided into two groups with split injection or splitless injection and determined by Headspace GC with FID. DB -624 capillary column（30 m × 530 μm, 3 μm） was used and the carrier gas was nitrogen gas. The seven kinds of residual solvents were separated completely by temperature program. RESULTS Under the two chromatographic conditions, the linearity, accuracy, precision and sensitivity of seven organic solvents met the authorized requirements. CONCLUSION The method is rapid and accurate, and can determine the seven kinds of residual organic solvents in ET -26 hydrochloride.