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机构地区:[1]广东食品药品职业学院,510520
出 处:《医学信息(下旬刊)》2009年第8期239-240,共2页Medical information
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.
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