GC法测定盐酸马尼地平中有机溶剂残留量

摘要

目的：建立测定盐酸马尼地平有机溶剂的气相方法。方法：采用Agilent DB-624毛细管柱（30 m×0.53 mm,3μm）;氮气为载气,压力为19 kPa;分流比为6∶1;进样口温度为170℃;FID检测器,检测器温度为210℃;程序升温：初始温度60℃,保持10 min,然后以20℃/min升至200℃,保持5 min。手动进样,平衡温度为60℃,以二甲基甲酰胺为溶剂,外标法测定盐酸马尼地平中甲醇的残留量。结果：在文章的色谱条件下,甲醇能得到良好的分离,空白对照无干扰,检测浓度在所考察的范围内与峰面积具有良好的线性,r=0.9984;平均回收率为104.20%,精密度试验与准确度试验RSD均小于2.0%,甲醇的检测限为21.0070μg/mL。结论：本试验建立的色谱方法简便、准确,适合盐酸马尼地平原料中有机溶剂残留量的检测。%Results： To establish a method of capillary gas chromatography for determination of residual solvents in manidipine hydrochloride.Methods： The residual solvents in manidipine hydrochloride were separated by Agilent DB-624 capillary（30 m×0.53 mm,3 um）column with an FID detector.The carried gas was nitrogen,the pressure was 19 kPa and the splitting-ratio was 6∶1.The injector temperature and the detector temperature were controlled at 170 ℃ and 210 ℃ respectively.The programmed column temperature was set as follows： maintained at 60 ℃ for 10 min and then raised to 200 ℃ at the rate of 20 ℃ min-1 followed by holding for 5 min.The containers of injector were in equilibrium at 60 ℃.The dimethylformamide（DMF） was used as solvent.Results： The detected solvents were separated completely.The calibration curve of solvent showed a good linear relationship（r=0.9984） with good precision and accuracy（RSDs were less than 2.0 %）.The average recovery rate was 104.20 %.The LOD of methanol was 21.0070 ug/mL.Conclusion： The established method is simple,ccurate,and can be used for the determination of residual solvents in manidipine hydrochloride.