摘要
建立了采用气相色谱法测定头孢噻肟钠样品中的残留溶媒丙酮、异丙醇含量的方法。采用气相色谱法,石英毛细管柱对头孢噻肟钠粉针剂中的主要残留溶剂丙酮、异丙醇进行分析,探索得到合适的色谱柱和溶剂以及色谱条件。实验以正丙醇为内标物,采用PEG-20M弹性石英熔融毛细管柱（30 m×0.25 mm×0.33μm）;载气为氮气,流量为1.14 m L/min,分流比为1∶20,初始柱温为60℃,保持时间为3 min,升温速率为10℃/min,终点温度为170℃,保持10 min;FID检测器温度为250℃;气化室温度为250℃。结果表明,丙酮、异丙醇在8~1 000μg/m L范围内与内标峰面积比有良好的线性关系（丙酮：r2=0.9997;异丙醇：r2=0.999 9）;回收率丙酮为97.7%,RSD=6.7%（n=9）;异丙醇回收率为89.6%,RSD=11.7%（n=9）。本法操作简便,结果准确,为有效控制头孢噻肟钠的残留溶媒建立了可靠的方法。
Based on gas chromatography and quartz capillary column, a method for determination of the main residue solvent of acetone and isopropanol in cefotaxime sodium was establishedl with n-propanol as the internal standard materia.PEG-20 M flexible fused silica capillary column（30 m × 0.25 mm × 0.33μm） was used as column. The other experimental conditions were carrier gas was nitrogen, its flow rate was 1.14 m L / min and split ratio 1∶20; initial column temperature was 60℃ and holding time was 3 min; heating rate was 10 ℃ / min; endpoint temperature was 170 ℃ and maintain time was 10 min; FID detector temperature was 250 ℃;gasification chamber temperature was 250 ℃. Results show that acetone and isopropyl alcohol in the range of 8 ~ 1 000μg / m L have good linear relationship with r2= 0.999 7（acetone） and r2= 0.999 9（isopropyl alcohol）;recovery yield of acetone is 97.7% and RSD = 6.7%（n = 9）,recovery yield of isopropanol is 89.6%, RSD = 11.7%,（n = 9）. This method is simple, accurate, and suitable for effective control the level of cefotaxime sodium residual solvents.
出处
《煤炭与化工》
CAS
2015年第4期38-43,共6页
Coal and Chemical Industry
关键词
头孢噻肟钠
丙酮
异丙醇
残留溶媒
气相色谱
cefotaxime
acetone
isopropanol
residual
solvent
gas chromatography
