毛细管GC测定石杉碱甲贴片中有机溶剂残留量

Determination of Residual Organic Solvents in Huperzine-A Patches by Capillary GC

目的:建立石杉碱甲贴片中异丙醇、乙酸乙酯残留量的测定方法。方法:采用毛细管气相色谱法,色谱柱为 HP-5(5%二苯基-95%二甲基聚硅氧烷);柱温:40℃。载气为氮气;检测器为 FID;外标法计算含量。结果:在该色谱条件下,测得乙酸乙酯和异丙醇两溶剂在2.50-12.5μg·mL^(-1)范围内线性均良好(r=0.9991和0.9994);平均回收率分别为96.57%和98.09%,RSD 分别为1.4%和1.7%;异丙醇、乙酸乙酯的最低检测限均为0.5 ng;10批样品中上述有机溶剂残留量均符合ICH 和 GMP 要求。结论:该毛细管气相色谱法灵敏、准确、可靠,适用于本品中有机溶剂残留量测定。

Objective：To determined the residual organic solvents （iso -propanol and ethyl acetate）in Huperzine-A patches. Methods：A capillary GC method was developed with HP -5 capillary column with FID detector and nitrogen as the carries gas. Results：The analytical validation for each of residual organic solvents was performed. The linearities were good between 2.50 - 12.5μg·mL^- 1 of both solvents （ r = 0. 9991 and 0. 9994 respectively）. The average recoveries were 96. 57% ,98.09% respectively with RSD of 1.4% and 1.7%. The limit of detection were both 0. 5 ng;The contents of residual organic solvents were detected with an external correlation method. The results in ten batches of samples were complied with the ICH or GMP requirements. Conclusions： This GC method is proved to be accurate, sensitive and reliable.