毛细管气相色谱法测定盐酸美金刚原料药中三氯甲烷的残留量

目的:建立毛细管气相色谱法测定盐酸美金刚原料药中三氯甲烷残留量的方法。方法:色谱柱为DB-1701石英毛细管柱,柱温采用程序升温,检测器为电子捕获检测器,检测器温度为250℃,进样口温度为200℃,以N,N-二甲基甲酰胺为溶剂。结果:三氯甲烷检测浓度线性范围为1.2～60μg·mL-(1r=0.9999);平均回收率为99.6%(RSD=0.8%);定量限为1.02pg;3批样品中三氯甲烷残留量均符合《中国药典》要求。结论:本方法简单、准确、灵敏度高、重复性好,可用于盐酸美金刚原料药中三氯甲烷残留量的测定。

Determination of Residual Chloroform in Memantine Hydrocloride Crude Material by Capillary Gas Chromatography

OBJECTIVE：To establish a capillary GC method for the determination of residual chloroform in memantine hydrocloride crude material. METHODS：Chloroform was determined on DB-1701 capillary column using temperature programming. ECD was used as detector with a temperature of 250 ℃. The inlet temperature was 200 ℃,and DMF was used as solvent. RESULTS：The linear range of chloroform was 1.2～60 μg·mL-1 （r=0.999 9）.The average recovery was 99.6% （RSD=0.8%）.The determination limit was 1.02 pg. The residual levels for chloroform in 3 batches samples were all up to the standard stipulated in Chinese Pharmacopeia. CONCLUSION：The method is simple,accurate,sensitive and reproducible,it can be used for the determination of residual chloroform in memantine hydrocloride crude material .