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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 establish a gas chromatographic method for the determination of related substances in memantine hydrochloride raw materials. Methods: A 50% -phenyl-methylpolysiloxane column (Agilent-DB-17, 30 m × 0.25 mm, 0.25 μm) -1 to 70 ° C for 42 min, 30 ° C · min-1 to 160 ° C for 15 min, 30 ° C · min -1 to 260 ° C for 10 min, carrier gas nitrogen The sample temperature was 250 ℃, the FID temperature was 280 ℃, the split ratio was 10:1, the flow rate was 2.5 mL · min -1, and the injection volume was 1 μL. Results: The impurities were completely separated from the main drug and 11 kinds of impurities. The linearity of each component was good in the range of 40% ~ 200%, r was greater than 0.99 and the average recovery was in the range of 50% ~ 150% All were 90% to 108% (n = 9) with RSD less than 5%. Conclusion: This method for the determination of memantine hydrochloride related substances, quantitative analysis of 11 impurities, simple and accurate operation, good reproducibility.