气相色谱法__(期刊论文)

气相色谱法测定头孢噻肟钠的残留溶媒

http://www.100md.com 《广东药学院学报》 2004年第1期

气相色谱法,,头孢噻肟钠；丙酮；异丙醇；残留溶媒；气相色谱,1仪器与试药,2实验与结果,讨论

     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OV1701弹性石英熔融毛细管柱(50 mm×0.25 mm×0.30 μm)。载气：氮气，流量1.2 mL/min，分流比1∶60；柱温(程序升温)：初始柱温45℃，保持时间3 min；升温速率20 ℃/min；终点温度105℃。FID检测器,温度250 ℃。气化室温度250 ℃。结果：丙酮、异丙醇在30～150 μg/mL范围内与内标峰面积比有良好的线性关系(丙酮：r=0.999 7；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，为有效控制头孢噻肟钠的残留溶媒建立了可靠的方法。

    关键词头孢噻肟钠；丙酮；异丙醇；残留溶媒；气相色谱

    Determination of residue solvent of acetone and isopropanol in cefotaxime sodium by gas chromatography

    LUO Yan-ping，CHEN Ning

    (Shenzhen GOSUN Pharmaceutical Co.,Ltd. Shenzhen, Guangdong 518049)

    Abstract 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. ......

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