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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 isopropyl ether in cefuroxime axetil. Methods The capillary column headspace method was used to determine the temperature by gas chromatography. The column was DB-624 capillary column (30.0 m × 0.320 m × 1.80 μm). Inlet temperature was 180 ℃. The temperature of hydrogen flame ionization detector (FID) was 220 ℃. The column temperature was programmed with an initial temperature of 80 ℃ for 3 min, and then ramped to 200 ℃ at a rate of 45 ℃ per minute for 3 min; carrier gas: high purity nitrogen; carrier gas flow rate: 3 mL · min -1. Headspace injection, the equilibrium temperature: 70 ℃, the balance of time 30 min. N, N-dimethylformamide as a dissolution medium. Results The solvent had no interference with the determination of residual solvents. The concentration of isopropyl ether showed a good linearity within the range of 0.025-2.5 mg · mL -1 with a correlation coefficient of 0.999 1. The recovery rate was 106.0%. Conclusion The method is simple, accurate, reproducible and can be used as a quality control measure to control residual isopropyl ether in cefuroxime axetil.