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目的:测定盐酸吉西他滨原料药中的有机溶剂残留量。方法:采用顶空气相色谱法,DB-624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。
Objective: To determine the residual amount of organic solvent in gemcitabine hydrochloride raw material. METHODS: The samples were separated by headspace gas chromatography (DB-624) on a silica capillary column (30m × 0.53mm, 3μm) at a vaporizer temperature of 250 ℃. The temperature of the flame ionization detector The initial column temperature was kept at 40 ℃ for 6min, the temperature was raised to 120 ℃ at 10 ℃ · min -1 and the temperature was raised to 230 ℃ at 40 ℃ · min -1 for 10min. The carrier gas was nitrogen. Results: The measured substances can be well separated, the peak area and concentration showed a good linear relationship. Conclusion: This method can be used as the raw material of gemcitabine hydrochloride organic solvent residues detected.