磺胺二甲嘧啶有机溶剂残留的GC测定
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[摘要] 目的:建立磺胺二甲嘧啶合成中所用有机溶剂丙酮残留量的测定方法。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(30 m×0.32 mm,0.5 μm),进样口温度160℃,检测器温度250℃,柱温 120℃,载气为氮气。结果:在该色谱条件下丙酮与二甲基亚砜能达到完全分离, 测得丙酮在2.08～6.25 μg/ml范围内线性关系良好(r=0.996 8),平均回收率分别为100.40% ( RSD=1.10%)。结论:该法简便、灵敏,易操作,可以作为磺胺二甲嘧啶原料药中有机溶剂残留量的检测。
[关键词] 磺胺二甲嘧啶;毛细管气相色谱法;残留有机溶剂
[中图分类号]R13 [文献标识码]A [文章编号]1673-7210(2009)07(c)-054-02
Determination of residual organic solvents in sulfadimidine by capillary GC
LIAO Hong
(Nanhai Beisha Pharmaceutical Company of Foshan City, Guangdong Province, Foshan 528244,China)
[Abstract] Objective: To develop a GC method for determination of acetone in sulfadimidine.Methods: Using Supelcowax-10 capillary column (30 m×0.32 mm, 0.5 μm),FID detector, the samples were dissolved in dimethyl sulfoxide, and sampling directly. The initial temperature was 120℃,the injection port and detector temperature were 160℃ and 250℃ respectively, using nitrogen as carrier gas ......
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