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目的采用顶空气相色谱法测定马来酸依那普利原料药中5种残留溶剂。方法色谱柱:DB624毛细管柱(氢火焰离子检测器),载气:氮气,进样口温度:220℃,检测器温度:220℃。柱温为程序升温:初始柱温为35℃,保持7 min,以每分钟20℃升至200℃,保持5 min。顶空条件:顶空平衡温度为80℃,平衡时间为20 min。正丙醇为内标物。结果 5种残留溶剂在各自的浓度范围内呈良好的线性关系(r=0.999 6～0.999 8,n=7),平均回收率(n=9)为84.24%～98.50%;精密度、重复性RSD均小于2%。结论本方法适用于马来酸依那普利中有机溶剂残留的测定。
Objective To determine five residual solvents in enalapril maleate by headspace gas chromatography. Methods Column: DB624 capillary column (flame ionization detector), carrier gas: nitrogen, inlet temperature: 220 ℃, detector temperature: 220 ℃. Column temperature for the program temperature: initial column temperature 35 ℃, hold 7 min, 20 ℃ per minute up to 200 ℃, hold 5 min. Headspace conditions: Headspace equilibrium temperature of 80 ° C, equilibration time of 20 min. Propanol as an internal standard. Results The five residual solvents showed a good linear relationship (r = 0.999 6 ~ 0.999 8, n = 7) and the average recoveries (n = 9) were 84.24% ~ 98.50% RSD less than 2%. Conclusion This method is suitable for the determination of organic solvents in enalapril maleate.