GC测定盐酸伊达比星原料药中的残留溶剂

GC Detection of Residual Solvents in Idarubicin Hydrochloride

关键词:  盐酸伊达比星  残留溶剂  气相色谱法  顶空进样

Key words:  idarubicin hydrochloride  residual solvents  GC  headspace

摘要:

目的 建立盐酸伊达比星原料药中残留溶剂的检查方法。方法 采用毛细管色谱柱顶空进样气相色谱程序升温法测定。色谱柱为DB-624石英毛细管柱(30.0 m×0.530 mm，3.00 mm)；进样口温度：200 ℃；氢火焰离子化检测器(FID)温度：250 ℃；柱温：程序升温，初始温度50 ℃，保持6 min，再以10 ℃·min^-1的升温速率升至165 ℃，维持2.5 min；载气：氮气；流速：4.0 mL·min^-1。顶空进样，平衡温度：105 ℃，平衡时间：20 min，进样体积：1.0 mL。以二甲基甲酰胺(DMF)为溶解介质。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，方法的精密度良好，各溶剂的回收率较为理想。结论 该法适用于盐酸伊达比星原料药的残留溶剂测定。

Abstract:

OBJECTIVE To establish a method for detection of the residual solvents in idarubicin hydrochloride substance. METHODS The residual solvents in this substance were determined by GC equipped with FID detector and linked with DB-624 capillary column (30.0 m×0.530 mm, 3.00 mm ). The carries gas was nitrogen. The inlet temperature was 200 ℃ and the FID detector temperature was 250 ℃. The column temperature rose by program: the initial temperature was 50℃, maintained for 6 min, raise to 165 ℃ with a rate of 10 ℃·min^-1, maintained for 2.5 min. The flow rate of carries gas N2 was 4.0 mL·min^-1. The heated temperature of the headspace oven was 105 ℃, the heated time lasted 20 min, and the injection volume was 1.0 mL. The dissolved medium used to prepare all of the test solutions was DMF. 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 detection of residual solvents in buflomedil hydrochloride substance.