克林霉素磷酸酯中有机溶剂残留量测定

Determination of Residual Organic Solvents in Clindamycin Phosphate

目的建立测定克林霉素磷酸酯中有机溶剂甲醇、乙醇、丙酮、1,2-二氯乙烷和吡啶残留量的顶空气相色谱法。方法采用AgilentHP-Innowax色谱柱(30 m×0.53 mm,1.0μm),载气为氮气,分流比1∶1,检测器FID温度280℃,柱温80℃,进样口温度200℃,顶空瓶温度80℃,平衡时间40 min。结果甲醇、乙醇、丙酮、1,2-二氯乙烷和吡啶5种溶剂的最低检测限分别为0.06,0.5,0.1,0.005,0.2μg/mL。结论顶空气相色谱法准确、简便、专属性强、重现性好,可作为该产品的质量控制方法。

Objective To develop a headspace capillary GC method for the determination of methanol,ethanol,acetone,1,2-dichloroethane and pyridine in clindamycin phosphate.Methods The residual solvents in clindamycin phosphate were separated by HP-Innowax capillary column（30 m × 0.53 mm,1.0 μm） with FID detector.The carried gas was nitrogen.The injector temperature and the detector temperature were controlled at 200 ℃ and 280 ℃ respectively.The column temperature was 80 ℃.The containers of headspace injector were in equilib-rium at 80 ℃ for 40 min,the splitting-ratio was 1 ∶ 1.Results The detection limits of methanol,ethanol,acetone,1,2-dichloroethane and pyridine were 0.06,0.5,0.1,0.005 and 0.2 μg/mL,respectively.Conclusion The method is simple with strong specificity and good repro-ducibility,which can be used for the determination of residual solvents in clindamycin phosphate.