顶空气相色谱法测定头孢曲松钠中有机溶剂的残留

目的:本文建立顶空气相色谱法测定头孢曲松钠样品中残留溶媒含量的方法。方法:实验以正丙醇为内标物,采用SPB-1弹性石英熔融毛细管柱(30m×0.25mm×1.0μm);载气:氮气,流量1.2mL/min;柱温(程序升温):初始柱温40℃,保持时间7min;升温速率8℃/min,终点温度120℃,保持时间5min;FID检测器,温度250℃;气化室温度200℃。结果:甲醇、乙醇、乙腈、丙酮、异丙醇、二氯甲烷、正丙醇、乙酸乙酯在一定浓度范围内峰面积有良好的线性关系(r0.999),加标回收率为97%～104%,相对标准偏差均小于1%,最低检出限小于0.5μg/L。结论:本法操作简便,结果准确,适用于头孢曲松钠中残留溶媒的分析确证。

Determination of Residual Solvents in Ceftriaxone Sodium by Head-Space Capillary Gas Chromatography

To establish a method of the head-space capillary gas chromatography for determination of residual solvents in ceftriaxone sodium. The test used 1-propanol as internal standard preparation and uses SPB-1 column （30m×0.25mm× 1.0μm）. Carrier gas： nitrogen,flow rate：1.2mL/min,rate of diversion：1：50; Temperature of column （temperature program）：temperature of string point： 40℃,retention time： 7min; rate of the rise f temperature：8℃/min; Temperature of the end point： 120℃,retention time：5min. The temperatures set for injector and FID detector were 200℃and 250℃ respectively. Result： within a certain extent,the peak area of methanol,ethanol,acetonitrile,acetone,iso-propanol,dichloromethane,ethyl acetate had a good linear （r0.999）,and the recoveries ranged from 97% to 104% with relative standard deviations between 0.41% and 0.90% for different residues. The limit of detection was less than 0.5μg/L for all the residue. Conclusion： this method was easy to operate with precise results,which established a reliable method for the control of residue solvent of ceftriaxone sodium.