顶空气相色谱法测定马来酸依那普利中5种残留溶剂

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。

Simultaneous determination of five residual solvents in enalapril maleate by headspace gas chromatography

Objective To develop a method for determination of five residual solvents in enalapril maleate by headspace gas chromatography. Methods The analysis was performed on a DB-624 capillary column and a flame ionization detector. The carrier gas was nitrogen. The temperatures for the injector and FID detector were 220 ℃. The programmed column temperature was as follows: starting at 35 ℃ for 7 min, and then rising to 200 ℃ at 20 ℃·min^-1 followed by holding for 5 min. The optimized equilibrium temperature was 80 ℃ and equilibrium time was 20 min. Results Linear responses were obtained for the residual of 5 kinds solvents in their respective concentration ranges (r=0.999 6-0.999 8,n=7). The rate of recovery (n=9) was in the range of 84.24%-98.50%. The RSD of precision and accuracy was less than 2%. Conclusion The method can be used for detection of the residual solvents in enalapril maleate.