毛细管气相色谱法测定盐酸美金刚有关物质  

GC determination of related substances in memantine hydrochloride

作　　者：陈玲[1] 骆雪芳[1] 钟文英[1] 

机构地区：[1]中国药科大学理学院,南京211198

出　　处：《中国新药杂志》2016年第10期1170-1176,共7页Chinese Journal of New Drugs

摘　　要：目的:建立气相色谱方法检测盐酸美金刚原料中有关物质。方法:采用50%-苯基-甲基聚硅氧烷柱(Agilent-DB-17,30 m×0.25 mm,0.25μm),程序升温(起始温度50℃,保持1 min,15℃·min-1升至70℃,保持42 min,30℃·min-1升至160℃,保持15 min,30℃·min^(-1)升至260℃,保持10 min),载气氮气,进样口温度250℃,FID温度280℃,分流比10∶1,流速2.5 m L·min^(-1),进样量1μL。结果:杂质与主药以及11种杂质之间均能完全分离,在限度40%~200%范围内,各组分线性良好,r均大于0.99,在限度50%~150%范围内平均回收率均在90%~108%(n=9),RSD均小于5%。结论:本法测定盐酸美金刚有关物质,能定量分析11种杂质,操作简便准确、重复性好。Objective： To develop a GC method for determination of related substances in memantine hydrochloride. Methods： A 50% phenyl-methylpolysiloxane capillary column（ Agilent DB-17,30 m × 0. 25 mm,0. 25 μm） was used with a programmed temperature procedure. Namely,the initial temperature was 50 ℃ for1 min,increased the temperature to 70 ℃ at 15 ℃·min^（- 1）and maintained for 42 min,increased the temperature to160 ℃ at 30 ℃·min^（- 1）and kept for 15 min,and then increased the temperature to 260 ℃ at 30 ℃·min^（- 1）and maintained for 10 min. The flow rate was 2. 5 m L·min- 1; nitrogen was used as carry gas; the temperature of SPL was 250 ℃; the temperature of FID was 280 ℃; the spilt ratio was 10; injection volume was 1 μL. Results： The satisfactory resolution was achieved between related substances and memantine hydrochloride. It showed a good linearity in the range of 40% to 200% of the limit concentration（ r〉 0. 99）. The average recovery（ n = 9） was in the range of 90% and 108%（ RSD〈 5%）. Conclusion： The developed method is suitable for the quantitative analysis of 11 related substances,and it is simple and accurate with high repeatability.

关 键 词：盐酸美金刚 有关物质 气相色谱法 

分 类 号：R971[医药卫生—药品]