顶空气相色谱法测定盐酸吉西他滨中的残留溶剂

目的：测定盐酸吉西他滨原料药中的有机溶剂残留量。方法：采用项空气相色谱法，DB击24石英毛细管柱（30m×0．53mm，3μm），汽化室温度250℃；氢火焰离子化检测器（FID）温度：300℃；柱温：程序升温，起始柱温为40℃，保持6min，以10％·min^-1升温至120℃。以40℃·min^-1升温至230℃保持10min；载气：氮气。结果：被测物质均能得到很好的分离，峰面积与浓度呈良好的线性关系。结论：该法可以作为盐酸吉西他滨原料药中有机溶剂残留量的检测。

Determination of Residual Solvents in Gemcitabine Hydrochloride by headspace gas chromatography

Objective： To establish a method for detection of residual solvents in gemcitabine hydrochloride. Method ： The residual solvents in gemcitabine hydrochloride was determined by headspace GC with DB-624 capillary column （30 m × 0.53mm,3μm） with FID detector and nitrogen as the carries gas. The injector temperature was 250℃ ,the detector temperature was 300℃ ,the column temperature rosed by program, the initial temperature was 40℃ and maintained for 6 min,rosed to 120℃ with a rate of 10℃·min^-1 ,then rosed to 230℃ with a rate of 400℃·min^-1 and maintained for 10min. Result： The solvents could be completely separated, and the calibration curves of each solvent had good linear relationship within a certain range. Conclusion： The method is proved accurate and reliable, it can be used for the determination of residual solvents in gemcitabine hydrochloride.