目的: 建立GC法测定3-氨基-1-金刚烷醇(VILS-03)中有关物质金刚烷胺、1,3-金刚烷二醇、1,3,5-金刚烷三醇、1,3,5,7-金刚烷四醇的含量。方法: 采用DB-1毛细管柱(50 m×0.53 mm×5 μm),进样口温度300 ℃,柱流速2.0 mL·min-1,进样方式用分流进样,分流比5∶1,载气为氮气,进样量为1 μL;外标法计算。结果: 空白溶剂均不干扰VILS-03有关物质的检测;金刚烷胺、1,3-金刚烷二醇、1,3,5-金刚烷三醇、1,3,5,7-金刚烷四醇均在一定范围内线性良好,r均>0.990;定量限分别为1.375、1.557、1.363、4.042 μg·mL-1;50%、100%、150%水平的加样回收率均良好。金刚烷胺平均加样回收率(n=3)分别为107.3%、107.3%、105.2%,RSD分别为0.67%、1.1%、2.3%。1,3-金刚烷二醇平均加样回收率(n=3)分别为93.6%、100.3%、95.6%,RSD分别为4.7%、1.6%、2.6%。1,3,5-金刚烷三醇平均加样回收率(n=3)分别为94.6%、96.7%、95.7%,RSD分别为1.9%、1.0%、2.4%。1,3,5,7-金刚烷四醇平均加样回收率(n=3)分别为95.1%、97.4%、99.5%,RSD分别为1.2%、0.63%、2.1%。室温条件下,对照品溶液和加标样品溶液在70.5、63 h内稳定性良好。3批次样品中,1,3-金刚烷二醇检出量分别为0.46%、0.36%、0.59%,其余杂质均未检出。结论: 该方法灵敏度高,专属性和准确度好,可用于VILS-03有关物质的检测。
Objective: To establish a method for the determination of amantadine, 1, 3-dihydroxyadamantane, 1,3,5-adamantanetriol and 1, 3, 5, 7-tetrahydroxyadamantane in 3-amino-1-adamantanol(VILS-03). Methods: An DB-1 capillary column(50 m×0.53 mm,5 μm) was used, the injector temperature was 300 ℃, and the flow rate of carries gas was 2.0 mL·min-1. The injection mode was split injection, and the split ratio was 5∶1, with nitrogen as the carrier gas. The injection volume was 1 μL, calculated by external standard method. Results: None of the blank solvents interfered with the detection of related substances of VILS-03, amantadine, 1, 3-dihydroxyadamantane,1, 3, 5-adamantanetriol and 1, 3, 5, 7-tetrahydroxyadamantane all had good linearity in a certain range, and r was greater than 0.990. Limit of quantitation(LOQ) were 1.375, 1.557, 1.363, 4.042 μg·mL-1. The recoveries of samples at 50%, 100%, and 150% levels were good. The average recoveries of amantadine (n=3) being 107.3%, 107.3%, and 105.2%; the RSD was 0.67%, 1.1%, and 2.3%, respectively. The average sample recoveries of 1, 3-dihydroxyadamantane (n=3) were 93.6%, 100.3%, and 95.6%; the RSDs were 4.7%, 1.6%, and 2.6%, respectively. The average sample recoveries (n=3) of 1,3,5-adamantanetriol were 94.6%, 96.7%, and 95.7%; the RSDs were 1.9%, 1.0%, and 2.4%, respectively. The average sample recoveries (n=3) of 1, 3, 5, 7-tetrahydroxyadamantane were 95.1%, 97.4%, and 99.5%; the RSDs were 1.2%, 0.63%, and 2.1%, respectively. The control solution and the labeled sample solution had good stability within 70.5 h and 63 h at room temperature. Test results showed that, except for 1, 3-dihydroxyadamantane detection amount of 0.46%, 0.36%, 0.59% respectively, other impurities were not detected in three batches of samples. Conclusion: The method has high sensitivity, specificity and accuracy, and can be used for the detection of VILS-03 related substances.
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