【摘要】 建立以正二十烷为内标物的气相色谱法,测定盐酸美金刚原料药的含量和有关物质。使用毛细管色谱柱(30 m×0.25 mm,0.5μm 50%-苯基-50%-甲基聚硅氧烷),程序升温(初始温度130℃,保持8 min;再以20℃/min的升温速率升至200℃,保持8 min;以相同速率降温至130℃,保持2min);载气为氮气(恒流),流速2.5 m L/min;分流比10∶1;进样口温度260℃;FID检测器温度260℃。结果表明:盐酸美金刚在0.2~2.0 mg/m L呈良好的线性关系,平均回收率100.9%,最低检测限100×10-6,降解产物和中间体均能与盐酸美金刚完全分离。该气相色谱内标法操作简单、结果准确、专属性好。更多还原

【Abstract】 Using n-eicosane as internal standard substance,gas chromatography( GC) internal standard method for assay memantine hydrochloride and related substances is established. The chromatographic procedure is carried out as follows: using a capillary column with 30 m long and 0. 25 mm in internal diameter coated with a film( 0. 5 μm) of 50% phenyl and 50% methylpolysiloxane; temperature programming( maintain the temperature of the column at 130 ℃ for 8 min,then raise to 200 ℃ at a rate of 20 ℃ / min,maintain at 200 ℃ for 8 min,reduce to 130 ℃at the same rate,maintain at 130 ℃ for 2 min); nitrogen as the carrier gas with a split ratio of 10∶ 1 and a flow rate of 2. 5 m L / min; maintain the injection port at 260 ℃ and FID detector at 260 ℃. The results show that the memantine hydrochloride has a good linearity in the range of 0. 2 to2. 0 mg / m L,the recovery rate is 100. 9%; the limit of detection is 100 ×10- 6. The degradation products and intermediates can be separated from memantine hydrochloride. The method is simple,accurate and specific.更多还原