顶空气相色谱法测定洛氟普啶中有机溶剂残留量

Determination of residual solvents in revaprazan by headspace GC

目的：建立顶空气相色谱法测定洛氟普啶中有机溶剂残留量。方法：采用Agilent DB-624毛细管柱（30 m×0.32 mm,1.8μm）;氮气为载气,流速为1.3 mL·min^-1;分流比为1∶1;进样口温度为200℃;FID检测器,检测器温度为250℃;程序升温：初始温度40℃,保持10 min,然后以30℃·min^-1升至240℃,保持5 min。顶空进样,平衡温度为100℃,平衡时间为30 min;以二甲基甲酰胺为溶剂,外标法测定洛氟普啶中甲醇、乙醇、丙酮和二氯甲烷的残留量。结果：在本文色谱条件下,甲醇、乙醇、丙酮和二氯甲烷均能得到良好的分离,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=0.9993-0.9996;平均回收率为93.8%-103.6%,精密度试验及准确度试验的RSD均小于2.0%,甲醇、乙醇、丙酮和二氯甲烷检测限分别为0.765,0.948,0.463,0.680μg·mL^-1。结论：本试验建立的色谱方法简便、准确,适合洛氟普啶原料中有机溶剂残留量的检测。

Objective：To establish a method of headspace capillary gas chromatography for the determination of residual solvents in revaprazan.Methods：The residual solvents in revaprazan were separated by Agilent DB-624 capillary（30 m×0.32 mm,1.8 μm）column with an FID detector.The carried gas was nitrogen,the flow rate was 1.3 mL·min-1 and the splitting-ratio was 1∶1.The injector temperature and the detector temperature were controlled at 200 ℃ and 250 ℃ respectively.The programmed column temperature was set as follows：maintained at 40 ℃ for 5 min and then raised to 200 ℃ at the rate of 30 ℃·min^-1 followed by holding for 5 min.The dimethylformamide（DMF）was used as solvent.The containers of head-space injector were in equilibrium at 100 ℃ for 30 min.Results：The detected solvents were separated completely.The calibration curve of each solvent showed a good linear relationship（r=0.9993-0.9996）with good precision and accuracy（RSDs were less than 2.0%）.The average recovery rate was in the range of 93.8%-103.6%.The LOD of methanol,ethanol,acetone and dichloromethane was 0.765,0.948,0.463,0.680 μg·mL^-1.Conclusion：The established method is simple,accurate,and can be used for the determination of residual solvents in revaprazan.