毛细管气相色谱法测定盐酸头孢唑兰有机溶剂残留量

CGC Determination of Residual Solvent in Cefozopran Hydrochloride

目的:建立毛细管气相色谱法测定盐酸头孢唑兰有机溶剂残留量。方法:色谱柱:采用气相色谱法测定,聚乙二醇为固定相的毛细管色谱柱(WAX 30.0 m×0.53 mm,1.0μm)(30.0 m×0.53 mm,1.0μm);载气为氮气。检测器温度:250℃;进样口温度:200℃;程序升温:初始温度50℃保持6 min,以15℃·min-1升温至180℃,保持5 min;顶空进样。平衡温度为70℃,平衡时间为30 min。分流比为1∶5,溶剂为二甲基亚砜。结果:被测物均能得到很好的分离,峰面积与浓度呈良好的线性关系,精密度良好。结论:该方法可用于盐酸头孢唑兰中有机溶剂残留量的检测。

Objective:To establish a method for determination of the residual solvents in Cefozopran Hydrochloride with head-space capillary gas chromatography(CGC).Methods:The residual solvents in Cefozopran Hydrochloride were separated by WAX capillary column(30.0 m×0.53 mm,1.0μm)with an FID detector.The carried gas was nitrogen.The injector temperature and detector temperature were controlled at 200℃and 250℃,respectively.The programmed column temperature was set as follows:maintained at 50℃for 6 min and then raised to 180℃at the rate of 15℃·min-1 followed by holding for 5 min.The sample was dissolved by indimethyl sulfoxide.The containers of head-space injector were in equilibrium at 70℃for 30 min and the splitting-ratio was 1∶5.Results:All the compounds were separated completely.The calibration curve of each compounds showed a good linear relationship with good precision and accuracy.Conclusion:The established method is accurate and reliable.It can be used for the determination of residual solvents in cefozopranhydrochloride.