摘要
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 headspace capillary GC method for determination residual solvents in Cefoperazone Sodium and Sulbactam Sodium for Injection. METHODS The residual solvents in this substance were determined by HS-GC equipped with FID detector and linked with DB624 capillary column (30.0m x 0.250mm x 1.4tsm). The inlet temperature was 23012 and the FID detector temperature was 250℃. The column temperature rose by program: the initial temperature was 3512, maintained for 5min, raise to 40℃ with a rate of 11℃ min- 1, maintained for 2rain, then raise to 6012 with a rate of 10℃ rain t maintained for 5rain, then raise to 18012 with a rate of 6012 rain-1, maintained for 4min. The carries gas was high pure nitrogen.The flow rate of carries gas N2 was 1.5mL rain- l. The heated temperature of the headspace oven was 70℃, the heated time lasted 30rain, and the injection volume was 1.0mL. The dissolved medium used to prepare all of the test solutions was water. RESULTS Each solvent could be completely separated, and the calibration curves of each solvent showed good linear relationship, precision and accuracy within a certain range.CONCLUSION The method is accurate and reliable. It can be applied in detection of residual solvents in Cefoperazone Sodium and Sulbactam Sodium for Injection.
出处
《海峡药学》
2012年第2期53-56,共4页
Strait Pharmaceutical Journal