气相色谱法测定盐酸美金刚胶囊的含量

目的: 建立盐酸美金刚胶囊剂含量测定的GC分析方法。方法: 样品先碱化后用甲苯萃取。色谱系统采用HP-5气相色谱柱(30 m×0.32 mm，膜厚0.25 μm)，柱温为程序升温，起始温度50℃，以20℃·min^-1的速率升至145℃，再以30℃·min^-1的速率升至250℃，保持5 min，氢火焰离子化检测器(FID)，分流比为10∶1。用盐酸金刚烷胺作为内标物，按内标法以峰面积计算。结果: 盐酸美金刚浓度在10~60 μg·mL^-1范围内，与主成分峰与内标峰面积比值呈良好的线性关系，r=0.9998；定量限(S/N=10)为4 ng；平均回收率(n=9)为99.8%；精密度RSD(n=6)为0.25%；重复性试验，样品含量的平均值(n=6)为102.3%，RSD为0.90%。结论: 该方法简单、准确，重复性好且专属性强，可用于盐酸美金刚胶囊剂的含量测定。

Objective: To establish a GC method for determination of memantine hydrochloride capsules. Methods: Samples were alkalified and then extracted with methylbenzene.The content of menantine hydrochloride was detected by FID after the separation in an HP-5 column (30 m×0.32 mm,film 0.25 μm).The column temperature was 50℃ at the beginning,and programmed to 145℃ at the rate of 20℃,then the temperature was elevated to 250℃ at the rate of 30℃,and then held for 5 min.The split flow was 10∶1.Amantadine hydrochloride was used as the internal standard,and methylbenzene was quantitatively determined by calculating the peak areas. Results: The calibration curve was linear over the range of 10-60 μg·mL^-1(r=0.9998);the limit of quantitation (S/N=10) was 4 ng;the average recovery (n=9) was 99.8%;RSD (n=6) of precision was 0.25%;the average content (n=6) of repeatability was 102.3% with RSD of 0.90%; the sample solution was relatively stable in 8 hours.Conclusion: The method is simple,accurate,reproducible and specific,which can be used for determination of memantine hydrochloridecapsules.

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