GC法测定盐酸金刚烷胺片中有关物质含量

Content Determination of Related Substances in Amantadine Hydrochloride Tablets by GC

目的:建立盐酸金刚烷胺片中有关物质的含量测定方法,并用于考察国内多批产品。方法:采用气相色谱(GC)法考察8个厂家41批盐酸金刚烷胺片中有关物质含量。色谱柱为HP-5;载气为氮气;氢火焰离子化检测器,进样口温度为200℃,检测器温度为300℃;柱温采用程序升温,初始温度为80℃,保持4min,然后以12℃.min-1升温至280℃,保持15min;载气流速为1.0mL·min-1;进样体积为2μL;内标为金刚烷。结果:盐酸金刚烷胺检测浓度线性范围为8.03～80.3mg.mL-(1r=0.9999);各破坏性分解产物均能与主峰分离,盐酸金刚烷胺最低检测限为0.22μg;8个厂家41批样品中均检测出有关物质,单个杂质量和杂质总量均在标准限度以下。结论:本方法准确、灵敏、可靠、专属性强,可有效控制盐酸金刚烷胺片的质量。

OBJECTIVE： To establish a method for the content determination of related substances in Amantadine hydrochloride tablets （AHT） so as to inspect multi-batches of AHT in China. METHODS： GC method was used to determine the contents of related substances in 41 batches of AHT from 8 manufacturers. The determination was performed on HP-5 column with an FID detector. The carried gas was nitrogen. The temperature of the injection port was maintaining at 200 ℃ and that of the detector at 300 ℃. The initial column temperature was 80℃, maintaining for 4 min, then raising to 280 ℃ at a rate of 12℃ ·min^-1 and mainmining it at 280 ℃ for 15 min. The flow rate of N2 was 1.0 mL·min^-1 and the injection volume was 2 μL. Diamantane was used as internal standard. RESULTS： The calibration curve showed a good linearity with the range of 8.03-80.3 mg· mL^-1 for amantadine hydrochloride （r=0.999 9）. The degradation substances could be separated from main peak. The lowest detectable limit of amantadine hydrochloride was 0.22 μg. Related substances could be found in 41 batches samples of 8 factories. Single impurity and total impurities of all batches samples were below limit. CONCLUSION： The method is accurate, sensitive, reliable and specific, and it can effectively control the quality of product.