摘要
目的 :建立了用气相色谱法测定头孢噻肟钠样品中的残留溶媒丙酮、异丙醇的含量的方法。实验以正丙醇为内标物 ,采用OV1 70 1弹性石英熔融毛细管柱 (5 0mm× 0 .2 5mm× 0 .30 μm)。载气 :氮气 ,流量 1 .2mL/min ,分流比 1∶6 0 ;柱温 (程序升温 ) :初始柱温 4 5℃ ,保持时间 3min ;升温速率 2 0℃ /min ;终点温度 1 0 5℃。FID检测器 ,温度 2 5 0℃。气化室温度 2 5 0℃。结果 :丙酮、异丙醇在 30～ 1 5 0 μg/mL范围内与内标峰面积比有良好的线性关系 (丙酮 :r =0 .9997;异丙醇 :r =0 9996 ) ;回收率 :丙酮为 99.7% ,RSD =1 .9% ,(n =9) ;异丙醇为 99.5 %RSD =2 .0 % ,(n =9)。结论 :本法操作简便 ,结果准确 。
To establish a method of the gas chromatography for determination of residue solvent of acetone and isopropanol in cefotaxime sodium. The test uses 1-propanol as internal standard preparation and uses OV1701column (50 mm×0.25 mm×0 3 μm). Carrier Gas: nitrogen, flow rate: 1 2 mL/min, rate of diversion: 1 ∶ 60; Temperature of column (temperature program): temperature of starting point: 45℃, retention time: 3min; rate of the rise of temperature: 20 ℃/min; temperature of end point: 105℃. FID detector at 250 ℃. Injector at 250 ℃. Result: within the range of 30～150μg/mL, the rate of peak area of acetone, isopropanol have a good linear proportion respectively with that of internal standard preparation (Acetone: r =0.999 7; isopropanol: r =0.999 6); rate of recovery: acetone 99.7% RSD=1.9%(n =9); isopropanol: 99.5% RSD=2.0%(n =9). Conclusion: this method is easy to operate with precise results, which establishes a reliable method for the control of residue solvent of cefotaxime sodium.
出处
《广东药学院学报》
CAS
2004年第1期16-18,共3页
Academic Journal of Guangdong College of Pharmacy
