顶空气相色谱法测定头孢曲松钠中三乙胺残留量

Determination of Residual Triethylamine in Ceftriaxone Sodium by Headspace Gas Chromatography Method

目的：建立顶空气相色谱法测定头孢曲松钠原料药中三乙胺残留量的方法。方法：以氢氧化钠溶液为溶剂,采用顶空毛细管气相色谱法,用DB-624毛细管柱进行梯度升温方式分离,以氮气为载气,氢火焰离子化检测器测定三乙胺残留量。结果：在上述色谱条件下三乙胺质量浓度在考察范围内与峰面积具有良好的线性关系（R^2=0.999）,平均回收率为98%~105%,精密度RSD均〈5%,最低检测限为0.03μg/ml,定量限为0.15μg/ml。结论：本法简单、灵敏、准确,适用于头孢曲松钠中三乙胺残留量的测定。

OBJECTIVE： To establish headspace gas chromatography method to determine residual triethylamine in ceftriaxone sodium（ CTR）.METHODS： Sodium hydroxide solution was set as solvent,headspace gas chromatography method was adopted,DB-624 capillary column separation was conducted with gradient heating way; and nitrogen was set as carrier gas,FID detector was used to detect the residual triethylamine.RESULTS： Under chromatographic conditions,the concentration of triethylamine within the scope of the investigation and the peak area were in good linear relationship（ R^2= 0.999）,the average recovery was 98%～105%,the precision of RSD 〈5%,with the lowest detection limit of 0.03 μg / ml and quantitative limit of 0.15 μg / ml.CONCLUSIONS： The method is simple,sensitive and accurate,suitable for the determination of residual triethylamine in ceftriaxone sodium.