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目的建立单硝酸异山梨酯中7种有机溶剂残留量的测定方法。方法顶空毛细管气相色谱法,DB-624柱(30m×0.32mm×1.8um),氢火焰离子化检测器(FID),以80%N,N-二甲基乙酰胺为溶剂,进样口温度150℃;检测器(FID)温度240℃;柱温:程序升温,初始温度50℃,保持5分钟,然后以每分钟10℃升至145℃,保持5分钟;顶空恒温箱温度85℃,传输管温度110℃,进样环温度105℃,加热20分钟。结果7种有机溶剂均达到完全分离,各成分线性试验所得回归方程,相关系数均在0.998以上,加样回收率均在94.4%～106.6%。结论经方法学试验验证,该方法准确、灵敏、可靠,可用于单硝酸异山梨酯原料药中7种残留溶剂的同时检测。
Objective To establish a method for the determination of 7 organic solvents in isosorbide mononitrate. Methods Headspace capillary gas chromatography, DB-624 column (30m × 0.32mm × 1.8um), flame ionization detector (FID) with 80% N, N-dimethylacetamide as solvent, Temperature: 150 ℃; FID: 240 ℃; Column temperature: programmed temperature, initial temperature: 50 ℃, hold for 5 minutes, then rise to 145 ℃ at 10 ℃ per minute for 5 minutes; , Transfer tube temperature 110 ℃, injection loop temperature 105 ℃, heating 20 minutes. Results All the seven organic solvents were completely separated. The regression equations obtained from the linear experiments of all the components were all above 0.998. The recoveries of the seven organic solvents ranged from 94.4% to 106.6%. Conclusions The method is validated by the methodological test. The method is accurate, sensitive and reliable and can be used for simultaneous determination of seven residual solvents in isosorbide mononitrate APIs.