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顶空气相色谱法测定头孢西丁钠原料中的残留溶剂 被引量:1

Analysis of residual solvents in raw material of cefoxitin sodium by headspace gas chromatography
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摘要 目的建立头孢西丁钠原料药中残留溶剂的测定方法。方法采用顶空进样毛细管气相色谱法;色谱条件:色谱柱为DB—624毛细管柱,程序升温方式:柱温初始为50℃,保持15 m in后,以30℃/m in的速度升温,升温至200℃,保持5 m in;氮气为载气,FID检测器。结果在设定的浓度范围内具有良好线性,甲醇、丙酮、二氯甲烷、乙酸乙酯、四氢呋喃的线性关系r分别为0.9998、0.9999、0.9999、0.9998、0.9986,平均回收率分别为95.65%、98.76%、92.41%、96.74%、93.95%(n=5)。结论方法准确,重现性好,灵敏度满意,适用于头孢西丁钠原料中残留溶剂的测定。 Objective To establish a method for determination of residue solvents in the raw material of cefoxitin sodium. Methods The headspace bottle was at 50 degrees C for 45min. The GC column was a 30.0 m × 0.32 mm × 1.4 μm stainless steel tube, The column temperature was 200 degrees C. Injection volume was 1 mL. Result The correlation coefficients of calibration curves of methanol, acetone, dichloromethane, ethyl acetate and tetrahydrofuran were 0. 9998, 0. 9999, 0. 9999,0. 9998 and 0, 9986, respectively. The average recoveries of methanol, acetone, dichloromethane, ethyl acetate and tetrahydrofuran were 95.65%, 98.76%, 92.41%, 96. 74% and 93.95% ( n = 5 ), respectively. Conclusion This method is simple and reliable for the quality control of the raw materials of cefoxitin sodium.
出处 《广东药学院学报》 CAS 2006年第2期160-161,163,共3页 Academic Journal of Guangdong College of Pharmacy
关键词 头孢西丁钠 残留溶剂 顶空气相色谱法 headspace gas chromatography cefoxitin sodium residue solvent
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