顶空气相色谱法测定头孢呋辛酯原料药中异丙醚的残留量

Determination of Isopropyl Ether in Cefuroxime Axetil by Head Space Gas Chromatography

目的建立头孢呋辛酯原料药中异丙醚残留量的测定方法。方法采用毛细管柱顶空进样法气相色谱程序升温法测定。色谱柱为DB-624毛细管柱(30.0 m×0.320 m×1.80μm);进样口温度:180℃;氢焰离子化检测器(FID)温度:220℃;柱温:程序升温,初始温度80℃,保持3 min,再以每分钟45℃的速度升温至200℃,维持3 min;载气:高纯氮气;载气流速:3 mL·min^(-1)。顶空进样,平衡温度:70℃,平衡时间30 min。以N,N-二甲基甲酰胺为溶解介质。结果溶媒对残留溶剂测定无干扰,异丙醚在0.025~2.5 mg·mL^(-1)浓度范围内呈现良好线性关系,相关系数为0.999 1。回收率为106.0%。结论该法操作简单,准确,重现性好,可作为控制头孢呋辛酯原料药中残留异丙醚的质控手段。

OBJECTIVE To establish a method for the determination of the residual volatile isopropyl ether in cefuroxime axetil. METHODS The isopropyl ether in the substance was determined by HS-GC equipped with FID detector and linked with DB-624 capillary column（30.0 m×0.320 m× 1.80 μm）.The inject temperature was 180 ℃ and the FID temperature was 220 ℃.The column temperature was rose by program ： the initial temperature was 80 %, maintained for 3 min, and then raise to 200 % with a rate of 45 ℃ · min-1 maintained for 3 min. The carried gas was high pure nitrogen. The flow rate was 3 mL-min-1. The heated temperature of the headspace oven was 70 %, and the heated time lasted for 30 min. The sample was dissolved in N, N-dimethylformamide. RESULTS The method proved to be linear in the ranges of 0.025 -2.5 mg· mL-1 and the average recovery was 106.0% for isopropyl ether. CONCLUSION This method is highly accurate and reliable, and is suitable for the determination of isopropyl ether in cefuroxime axetil.