气相色谱内标法测定盐酸美金刚含量和有关物质

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×0.25mm,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8min;以相同速率降温至130℃,保持2 min）;载气为氮气（恒流）,流速2.5 mL/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0.2～2.0mg/mL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.

Gas chromatography internal standard method for assay memantine hydrochloride and related substances

μUsing 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. 5μm） 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 mL/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 to 2. 0 mg/mL, the recovery rate is 100. 9% ; the limit of detection is 100× 10^-6. The degradation products and intermediates can be separated from memantine hydroehloride. The method is simple, accurate and specific.