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目的建立顶空毛细管气相色谱法,用于注射用头孢哌酮钠舒巴坦钠中14种残留溶剂的测定。方法采用毛细管柱顶空进样气相色谱程序升温法测定。色谱柱为DB-624弹性石英毛细管柱(30.0m×0.250mm×1.4μm);进样口温度:230℃;氢火焰离子化检测器(FID)温度:250℃;柱温:程序升温,初始温度35℃,保持5min,再以1℃.min-1的升温速率升至40℃,维持2min,再以10℃.min-1的升温速率升至60℃,维持5min,再以60℃.min-1的升温速率升至180℃,维持4min;载气:高纯度氮气;流速:1.5mL.min-1。顶空进样,平衡温度:70℃,平衡时间:30min,进样体积:1.0min。以水为溶解介质。结果被测各溶剂均能良好分离,各溶剂峰面积与浓度均呈良好的线性关系;方法的精密度良好;回收率较为理想。结论该法适用于注射用头孢哌酮钠舒巴坦钠的残留溶剂的检测。
Objective To establish a capillary gas chromatographic method for the determination of 14 residual solvents in cefoperazone sodium and sulbactam sodium for injection. Methods The capillary column headspace GC was used to determine the temperature. The column was DB-624 elastic quartz capillary column (30.0m × 0.250mm × 1.4μm); inlet temperature was 230 ℃; hydrogen flame ionization detector (FID) temperature was 250 ℃; column temperature was programmed temperature, The temperature was 35 ° C and kept for 5 min. The temperature was raised to 40 ° C at the temperature rising rate of 1 ° C-min-1 for 2 minutes and then raised to 60 ° C at the temperature rising rate of 10 ° C-min-1 for 5 minutes and then 60 ° C. min-1 heating rate rose to 180 ℃, maintaining 4min; carrier gas: high purity nitrogen; flow rate: 1.5mL.min-1. Headspace injection, equilibrium temperature: 70 ℃, equilibration time: 30min, injection volume: 1.0min. With water as the dissolution medium. Results The tested solvents could be separated well. The peak area and concentration of each solvent showed a good linear relationship. The precision of the method was good and the recovery rate was satisfactory. Conclusion This method is suitable for the determination of residual solvents in cefoperazone sodium and sulbactam sodium for injection.