顶空毛细管气相色谱法测定胸腺五肽长效微球中的残留溶剂

Determination of residual solvents in thymopentin continuous release microspheres by head-space capillary gas chromatography

目的:建立顶空毛细管气相色谱法,用于胸腺五肽长效微球残留溶剂的测定。方法:采用DB-624弹性石英毛细管柱(30 m×0.32 mm,1.8μm),载气为氮气,氢火焰离子化检测器,进样口及检测器温度均为250℃。柱温采用程序升温:初始温度为40℃,保持10 min,以8℃·min^(-1)升至120℃,保持4 min,再以40℃·min^(-1)升至200℃,保持2 min;流速为1.0 mL·min^(-1)。分流比为10:1,以二甲基亚砜为溶剂。结果:甲醇、乙醇、丙酮、乙腈、二氯甲烷、乙酸乙酯与四氢呋喃7种溶剂均得到了较好的分离;在各自浓度范围内均具有良好线性关系,测定精密度RSD均小于2%,标准加样回收率为97.6%～99.1%,RSD小于1.8%;制备的微球有机溶剂残留量符合中国药典限度要求。结论:方法准确可靠,可用于胸腺五肽长效微球中残留溶剂的测定。

Objective：To establish a head -space capillary GC method for determination residual solvents in thymopentin continuous release microspheres. Methods ： The analytical column was DB - 624 （ 30m 0. 32mm, 1.8 m）. The carrier gas was nitrogen, detector was FID. The injector and detector temperature was 250 ℃. The column temperature program was raised. The solvent was dimethyl sulfoxide. Results： Methanol, ethanol, acetone, acetonitrile, dichloromethane, ethyl acetate and Tetrahvdrofuran were completely separated. The calibration curve of each solvent showed good linear relationship, precision and accuracy. The average recovery were 97.6% -99. 1% （RSD 〈 1.8 % ）. The solvents residual in products are less than ChP 2005. Conclusion ： The method is simple, rapid and precise, it can be used for the determination of residual solvents in the TP - 5/PLGA Mierospheres.