摘要
目的:用毛细管柱气相色谱法建立测定盐酸美金刚原料药中二氯甲烷、乙腈、乙醚、乙醇的残留量的方法。方法:采用内壁涂有5%苯基-95%聚二甲基硅氧烷的毛细管柱(DB-5毛细管色谱柱30m×0.53mm×1.5μm),以氮气为载气,流速1.0ml/min。柱温箱:50℃保持12min,然后以30℃/min升温至230℃,至少保持12分钟。分流直接进样,进样口温度230℃,进样量:1.0μl。FID检测器,检测器温度280℃。按内标法计算残留溶剂的含量。结果:在考察的浓度范围内呈现良好的线性关系(二氯甲烷r=0.99885、乙腈r=0.99975、乙醚r=0.99659、乙醇r=0.99985),方法的精密度良好,回收率较为理想。结论:该法适用于盐酸美金刚原料药中二氯甲烷、乙腈、乙醚、乙醇的残留量的检测。
Objective： To establish a method for the determination of the residual solvents in memantine hydrochloride. Methods：The capillary was DB-5 （30m ×0.53mm ×1.5？m）.The carrier gas was nitrogen gas and FID was as detector. The injector temperature was 230℃ and the detector temperature was 280℃. The column temperature program was initial 50℃ （hold 12 min）,with the increase rate of 30℃ ·min-lto 230℃ （hold at least 12 min）.The assay of residual solvents were calculated by internal standard method. Results： It appeared a good linearity in the experimented concentration （r=-0. 99659-0.99985）. The precision of the method is good.The recovery rate of is ideal. Conclusions：The method is simple, sensitive accurate , and can be used for detection of four residual solvents （Methylene chloride,Acetonitrile,Ethyl ether, Ethanol） in memantine hydrochloride.
出处
《福建分析测试》
CAS
2012年第4期57-59,共3页
Fujian Analysis & Testing
