静态顶空气相色谱法测定苯磺酸氨氯地平中的溶剂残留量

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。

Static headspace gas chromatographic method for quantitative determination of residual solvents in amlodipine besylate

Objective To develop a method for determination of residual solvents in amlodipine besylate by static headspace gas chromatography. Methods Nitrogen gas was used as carrier gas. FID was used as detector. Ethyl acetate, isopropanol and methylbenzene were separated on DB-WAX (30 m×0.32 mm, 0.25 m) capillary chromatographic column using temperature programming and the solvent was dimethylformamide. N, N-dimethylacetamide was separated on DB-624 (30 m×0.25 mm, 1.4 μm) capillary chromatographic column using temperature programming and the solvent was N-methyl-2-pyrrolidone. Results The good linear relation of ethyl acetate, isopropanol, methylbenzene, N, N-dimethylacetamide were achieved within the investigated concentration range and r were from 0.997 0 to 0.999 9. The average recoveries were ranged from 101.8% to 103.9%. The limit of detection were separately 3.50, 6.01, 1.90, 13.3 mg•L-1. Conclusions The method is simple, sensitive, accurate and reproducible. It can be used for detection of residual solvents in amlodipine besylate in practical production.