磺胺二甲嘧啶有机溶剂残留GC测定.docVIP

磺胺二甲嘧啶有机溶剂残留GC测定 　　[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. Results: In these chromatographic conditions, acetone and dimethyl sulfoxide were completely separated. The calibration curve was linear in the range of 2.08-6.25 μg/ml(r=0.996 8).The average recovery was 100.40%,with RSD of 1.10%.Conclusion: The method is rapid, sensitive, precise with good reproducibility. It is suitable for the determination of residualorganic solvents in sulfadimidine API. 　　[Key words] Sulfadimidine; Capillary gas chromatography; Residual organic solvents 　　 　　磺胺二甲嘧啶化学名为N-(4,6-二甲基-2-嘧啶基)-4-氨基苯磺酰胺。磺胺二甲嘧啶是一种广谱抗菌药,它对多数革兰阳性菌和革兰阴性菌具有体外抗菌活性。由于磺胺二甲嘧啶在合成中使用了丙酮,根据[ICH]指导原则[1]、美国药典29版(USP29)[2]及中国药典2005版[3]的规定,原料药在合成中,所用过的有机溶剂都应对其最终产物进行残留溶剂的检测,故对丙酮加以检测和控制。参考有关文献[5-9],本实验采用溶液直接进样毛细管气相色谱法对磺胺二甲嘧啶残留的丙酮进行检测。结果表明,方法简便、重现性好、检测准确可靠。 　　1 仪器与试药 　　GC-17A气相色谱仪(SHIMADZU公司),磺胺二甲嘧啶(佛山市南海北沙制药有限公司,批号:210610001、210610002、210610003),丙酮对照品(广州化学制剂厂2),二甲基亚砜均为色谱纯。 　　2 方法和结果 　　2.1 色谱条件 　　色谱柱:Supelcowax-10(30 m×0.32 mm,0.5 μm);载气:氮气;检测器:氢火焰离子化检测器(FID);进样口温度160℃;检测器温度250℃;柱温120℃;溶液直接进样,分流比5∶1,