顶空毛细管气相色谱法测定阿折地平中的溶剂残留

摘 要 目的:建立顶空毛细管气相色谱法测定阿折地平中有机溶剂残留量的方法。方法: 采用CP-624毛细管色谱柱（30 m×0.32 mm，8 μm）；载气为氮气，进样口温度为200℃；FID检测器，检测器温度为250℃；柱温采取程序升温，起始温度 55℃，保持8 min，然后以10℃·min^-1的升至195℃，持续10 min。顶空进样，平衡温度为90℃，平衡时间为30 min；以二甲亚砜为溶剂，测定阿折地平原料药中乙醇、乙腈、乙酸乙酯和甲苯的残留量。结果:在本文的色谱条件下，各有机溶剂均能得到有效分离，在所考察的浓度范围内线性关系良好，r=0.997 0～0.999 0，平均回收率为95.4%～98.7%。结论:本方法灵敏、准确、可靠，可用于阿折地平中残留溶剂的检测。

Determination of Residual Solvents in Azelnidipine by Headspace Gas Chromatography

Objective： To establish a method of headspace capillary gas chromatography for the determination of residual solvents in azelnidipine. Method： The residual solvents in azelnidipine were separated by CP-624 capillary （30 m × 0.32 mm ,8 μm）column with an FID detector. The carried gas was nitrogen. The injector temperature and the detector temperature were controlled at 200℃ and 250℃, respectively. The programmed column temperature was set as follows ： maintained at 55℃ for 8 min and then raised to 195℃ at the rate of 10℃ ·min^-1 followed by holding for 10 min. The dimethyl sulfoxide （DMSO） was used as the solvent. The containers of headspace injector were in equilibrium for 30 min at 90%. Result： The detected solvents were separated completely. The calibration curve of each solvent showed a good linear relationship（ r = 0. 997 0-0.999 0 ）. The average recovery was within the range of 95.4% - 98.7%. Conclusion ： The established method is simple and accurate, and can be used for the determination of residual solvents in azelnidipine.