摘要
目的：建立磺胺二甲嘧啶合成中所用丙酮有机溶剂残留量测定方法。方法：采用毛细管气相色谱法，溶液直接进样，氢火焰离子化检测器（FID），以二甲基亚砜为溶剂，色谱柱为Supelcowax-10（30m×0．32mm×0．5μm），进样口温度160℃，检测器温度250℃，柱温120℃，栽气为氮气。结果：在该色谱条件下丙酮与二甲基亚砜能达到完全分离，测得丙酮线性试验所得回收方程相关系数在0．9968％，加样回收率分别为98．5％-102．8％，RSD〈2．0％。结论：该法可以作为磺胺二甲嘧啶原料药中有机溶剂残留量的检测。
Objective： To develop a GC method for determination of acetone in sulfadimidine. Method： Using Supelcowax- 10 capillary column （30m×0.32mm×0.5μm）, FID detector, the samples were dissolved in dimethyl sulphoxide, and sampling directly. The initial temperature was 120℃ ,the injection port and detector temperature were 160℃ and 250℃ respectively, using Nitrogen gas as carrier gas. Result： In these chromatographic conditions acetone and dimethyl sulphoxide were completely separated. The correlated coefficient of calibration curve of acetone in equation was 0. 9968%. The recoveries were between 95. 8% and 102.8%, RSD〈2.0%. Conclusion： The method is proved to be accurate and sensitive after validation. It is suitable for the determination of residual organic solvents in sulfadimidine API.
