摘要
目的建立顶空进样气相色谱法检测阿洛西林钠原料药中残留溶剂的方法。方法采用程序升温法测定。色谱柱为Agilent HP-1弹性石英毛细管柱(30.0 m×0.25 mm×1.00-m);进样口温度:200℃;氢火焰离子化检测器温度:250℃;柱温:程序升温,初始温度30℃,保持7 min,再以50℃.min-1的速率升至180℃,维持5 min;载气:氮气;流速:2.0 mL.min-1。顶空进样,顶空平衡温度:85℃,顶空平衡时间:30 min;进样体积:1.0 mL;以水为溶解介质;以丁酮为内标,测定了阿洛西林钠中5种溶剂的残留量。结果各被测溶剂均能良好分离,各溶剂峰面积与浓度均呈良好的线性关系,方法精密度良好,回收率均较为理想。结论该法适用于阿洛西林钠原料药中残留溶剂的测定。
OBJECTIVE To establish a method for determination of residual solvents in azlocillin sodium.METHODS The residual solvents in this substance were determined by GC equipped with FID detector and linked with Agilent HP-1 capillary column（30.0 m×0.25 mm×1.00 mm）.The inlet temperature was 200 ℃ and the FID detector temperature was 250 ℃.The column temperature rose by program： the initial temperature was 30 ℃,maintained for 7 min,raise to 180 ℃ with a rate of 50 ℃·min-1,maintained for 5 min.The carries gas was nitrogen and the flow rate of carries gas was 2.0 mL·min-1.The heated temperature of the headspace oven was 85 ℃,the heated time lasted 30 min,and the injection volume was 1.0 mL.The dissolved medium used was water and the internal standard was butanone.RESULTS Each solvent could be completely separated in chromatogram obtained from systemic suitability test,and the calibration curves of each solvent had good linear relationship within a certain range.CONCLUSION The method is accurate and reliable.It can be applied in determination of residual solvents in azlocillin sodium.
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2011年第11期1047-1050,共4页
Chinese Journal of Modern Applied Pharmacy
