摘要
目的:建立盐酸美金刚分散片含量及含量均匀度的GC测定法。方法:样品用水溶解,氢氧化钠溶液碱化,二氯甲烷萃取。色谱系统采用HP-5气相色谱柱(50 m×0.32 mm,1.05μm);柱温为程序升温,起始温度为120℃,维持3 min,以10℃·min^(-1)的速率升温至220℃,维持7 min;采用氢火焰离子化检测器(FID);分流比为1∶1;进样口温度为230℃;检测器温度为260℃;进样量为1μl;载气为高纯氮;流速为3.0 ml·min^(-1)。以金刚烷为内标物,采用内标法以峰面积进行计算。结果:盐酸美金刚在0.05~1.0 mg·ml^(-1)浓度范围内和主成分与内标峰面积的比值呈良好的线性关系(r=0.999 7);检测限和定量限分别为1.1 ng和3.3 ng;平均回收率为100.2%(RSD=0.73%,n=9)。结论:该方法操作简便,萃取过程毒性小,对环境污染小,且结果准确、精密度高、专属性强,可用于盐酸美金刚分散片含量及含量均匀度的测定。
Objective： To establish a GC method for the determination of content and content uniformity of memantine hydrochloride dispersible tablets. Methods： The sample was dissolved in water, alkalified by sodium hydroxide solution and extracted by methylene chloride. An HP-5 gas chromatography column （50 m × 0.32 mm, 1.05 μm） was used. The column temperature was programming increased, and the initial temperature maintained at 120 ℃ for 3 min, and then raised to 220℃ at a rate of 10℃ ·min^-1 and maintained for 7 rain. A hydrogerr flame ionization detector （FID） was used and the split ratio was 1 ： 1. The inlet temperature was 230 ℃ and the detector temperature was 260℃. The injection volume was 1 μl and the carrier gas was nitrogen with high purity at a flow rate of 3.0 ml ·min-1. Adamantane was used as the internal standard, and the internal standard method was used for the calculation. Results ： The calibration curve was linear over the range of 0.05-1.0 mg ·ml ^- 1 （ r = 0.999 7 ）. The detection limit and the limit of quantification was 1.1 ng and 3.3 ng, respectively. The average recovery was 100.2% （RSD =0.73% , n =9）. Conclusion： The method has the advantages of simple operation, small extraction process toxicity, little environmental pollution, high accuracy and high specificity, and can be used for the determination of content and content uniformity of memantine hydrochloride dispersible tablets.
出处
《中国药师》
CAS
2017年第5期935-937,共3页
China Pharmacist
