论文部分内容阅读
目的建立静态顶空气相色谱法测定苯磺酸氨氯地平中有机溶剂残留量的方法。方法采用静态顶空气相色谱法。检测器为氢火焰离子化检测器,载气为氮气,柱温为程序升温。采用DB-WAX(30 m×0.32 mm,0.25μm)毛细管色谱柱,以N,N-二甲基甲酰胺为溶剂,检测了苯磺酸氨氯地平中乙酸乙酯、异丙醇及甲苯的含量;采用DB-624(30 m×0.25 mm,1.4μm)毛细管色谱柱,以N-甲基吡咯烷酮为溶剂,检测了苯磺酸氨氯地平中N,N-二甲基乙酰胺的含量。结果乙酸乙酯、异丙醇、甲苯及N,N-二甲基乙酰胺在考察范围内线性关系良好,r为0.997 0～0.999 9,平均回收率为101.8%～103.9%,检测限分别为3.50、6.01、1.90和13.3 mg·L-1。结论本方法操作简单、灵敏、准确、重现性好,可用于实际生产中苯磺酸氨氯地平残留溶剂的检查。
Objective To establish a method for the determination of residual organic solvents in amlodipine besylate by static headspace gas chromatography. Methods Static headspace gas chromatography was used. The detector is a hydrogen flame ionization detector, the carrier gas is nitrogen, the column temperature for the program temperature. A DB-WAX (30 m × 0.32 mm, 0.25 μm) capillary column was used for the determination of amlodipine besylate in acetonitrile and isopropanol and toluene using N, N-dimethylformamide as solvent The content of N, N-dimethylacetamide in amlodipine besylate was determined by capillary column DB-624 (30 m × 0.25 mm, 1.4 μm) with N-methylpyrrolidone as solvent. Results The calibration curves of ethyl acetate, isopropanol, toluene and N, N-dimethylacetamide showed good linearity in the range of 0.997 0-0.9999 with the average recoveries of 101.8% -103.9%. The detection limits were 3.50, 6.01, 1.90 and 13.3 mg · L -1, respectively. Conclusion The method is simple, sensitive, accurate and reproducible. It can be used for the determination of residual amlodipine besylate in actual production.