毛细管气相色谱法检测头孢西丁钠原料药中的残留溶剂

Determination of residual solvents in active pharmaceutical ingredient of Cefoxitin Sodium by capillary gas chromatography(CGC)

目的建立气相色谱法测定头孢西丁钠原料药中的有机残留溶剂乙醇、丙酮及乙酸乙酯。方法色谱柱为HP-5(30m×0.53mm×1.5μm),载气为氮气,进样器温度为180℃,火焰离子检测器(FID)温度为250℃,柱温为50℃,以水为溶剂,进样量1μl。结果乙醇、丙酮及乙酸乙酯的线性关系r分别为0.9998、0.999及0.997,平均回收率分别为98.6%、102.6%及101.9%,最小检出量分别为6.0E～4ng、2.9E～4ng及3.1E～4ng。3批样品中均检测出丙酮残留,而未检出乙醇和乙酸乙酯。结论该方法高效、灵敏、准确,适用于同时检测头孢西丁钠原料药中有机残留溶剂乙醇、丙酮及乙酸乙酯的含量。

Objective To establish CGC to determine the residual solvents in active pharmaceutical ingredient of cefoxitin sodium,such as ethanol,acetone and ethyl acetate.Methods The HP-5（30m×0.53mm×1.5μm） column was adopted,and nitrogen gas was used as carrier.The temperature of the sampler,flame ionization detector（FID） and column was 180℃,250℃,50℃ respectively.The solvent was water,and the injecting volume was 1μL.Results The linear correlation （r） of ethanol,acetone and ethyl acetate was respectively 0.9998,0.999,0.997,the average recovery rate were respectively 98.6%,102.6%,101.9% and the minimum detectable amount were respectively 6.0E-4ng,2.9E-4ng and 3.1E-4ng.The acetone was detected from all the samples,but no ethanol and ethyl acetate could be detected.Conclusion The method was rapid, sensitive and accurate,and can be used for the determination of the content of residual organic solvents in active pharmaceutical ingredient of cefoxitin sodium at the same time,such as ethanol,acetone and ethyl acetate.