毛细管气相色谱法测定盐酸头孢他美酯中残留溶剂

Determination of Residual Solvents in Cefetamet Pivoxil Hydrochloride with Capillary Gas Chromatography

目的建立顶空进样和直接进样毛细管气相色谱法测定盐酸头孢他美酯中的残留溶剂。方法异丙醇、乙酸乙酯、丙酮测定采用顶空进样法,色谱柱:HP-INNOWAX PEG-20M毛细管柱(30.0 m×320μm,0.25μm),柱温为50℃,维持5 min,以每分钟30℃速率升至200℃,维持3 min,二甲亚砜为溶剂;二甲基甲酰胺测定采用直接进样法,色谱柱为DB-624(6%氰丙基苯基-94%二甲基聚硅氧烷固定液)石英毛细管柱(30.0 m×0.53 mm,3.0μm),柱温为100℃,维持6 min,以每分钟30℃速率升至200℃,维持5 min,二甲亚砜为溶剂。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,精密度和回收率良好。结论该法可用于盐酸头孢他美酯原料药中残留溶剂的检测。

Objective To establish a method for determination of residual solvents in cefetamet pivoxil hydrochloride by capillary gas chromatography（CGC） with head-space and direct sample adding system. Methods The isopropanol,ethyl acetate and acetone in cefetamet pivoxil hydrochloride were separated by HP-INNOWAX PEG-20M capillary column（30.0 m×320 μm,0.25 μm）through head-space injection.The column temperature was maintained at 50 ℃ for 5 min,then was raised to 200 ℃ at the rate of 30 ℃·min-1 and maintained at 200 ℃ for 3 min.The sample was dissolved in dimethyl sulfoxide.The dimethylformamide in cefetamet pivoxil hydrochloride were separated by DB-624 capillary column（30.0 m×0.53 mm,3.0 μm）through direct injection.The column temperature was maintained at100 ℃ for 6 min,then was raised to 200 ℃ at the rate of 30 ℃·min-1 and maintained at 200 ℃ for 5 min.The sample was dissolved in dimethyl sulfoxide. Results The measured solvents were separated completely.The calibration curve of each solvent showed a good linear relationship with precision and accuracy. Conclusion The established method is accurate and reliable,which can be used for determination of residual solvents in cefetamet pivoxil hydrochloride.