顶空毛细管气相色谱法测定富马酸阿奇霉素中的残留溶剂

CGC determination of residual solvents in azithromycin fumarate

目的建立毛细管气相色谱方法测定富马酸阿奇霉素中的残留溶剂。方法采用气相色谱法测定,色谱柱为:DB-5(5%苯基-95%二甲基硅氧烷固定液)石英毛细管柱(Agilent 60m×0.320mm×1.00μm),载气为氮气;柱温为60℃;FID检测器温度为250℃;进样口温度为200℃;顶空瓶平衡温度55℃,平衡时间30min。结果被测物均能得到良好的分离,峰面积与浓度呈良好的线性关系,精密度与回收率良好。结论该法可用于富马酸阿奇霉素原料中残留溶剂的检查。

Objective To establish a method of headspace capillary gas chromatography（CGC） for determination the residual solvents in azithromycin fumarate. Methods The residual solvents in azithromycin fumarate were separated by DB-5 capillary column（Agilent 60m×0.320mm× 1.00μm） with an FID detection. The carried gas was nitrogen. The column temperature was 60℃. The injector temperature and the detector temperature was controlled at 200℃ and 250℃, respectively. The containers of headspace injector were in equilibrium at 55 ℃ for 30min. Results The measured solvents were separated completely. The calibration curve of each solvent showed a good linear relationship with good precision and accuracy. Conclusion The established method was accurate and reliable. It can be used for the determination of residual solvent in azithromycin fumarate.