摘要
采用顶空气相色谱法测定罗氟司特原料药中残留溶剂甲醇、丙酮、乙腈、二氯甲烷、乙酸乙酯、甲苯和N,N-二甲基甲酰胺的含量。在DB-624毛细管色谱柱(30 m×0.32 mm×1.80μm)上,以高纯氮气为载气,检测器为氢火焰离子化检测器,进样口温度为220℃,检测器温度为250℃,以程序升温方式使甲醇、丙酮、乙腈、二氯甲烷、乙酸乙酯、甲苯和N,N-二甲基甲酰胺达到了完全分离。结果表明,7种溶剂在对应于限度的50%～150%浓度范围内具有较好的线性关系(R2≥0.99),重复性RSD为1.8%～3.7%,平均回收率为94.9%～108.0%,检测灵敏度均达到了预定的分析要求,在罗氟司特原料药中仅检测出甲醇和丙酮。该方法简便灵敏、准确可靠,适用于罗氟司特原料药质量控制中的残留溶剂检查。
A method for determining the residual solvents in roflumilast by headspace gas chromatography was established.The determination was carried out on the DB-624 capillary column（30 m×0.32 mm×1.80 μm） with FID detector sequential increase of temperature programming.The carrier gas was nitrogen,the injector temperature was 220 ℃,and the detector temperature was 250 ℃ with sequential increase of temperature programming.The residual solvents methanol,acetone,acetonitrile,dichloromethane,ethyl acetate,toluene and N,N-dimethyl formamide were separated completely.The results showed that the correlation coefficients of linearity was more than 0.99% for the seven residual solvents within the concentration of 50% to 150% of relative individual limit specified,the RSD of repeatability ranged from 1.8% to 3.7%,the average accuracy ranged from 94.9% to 108.0%.And the sensitivity was complied with the predefined analytical requirements.Methanol and acetone were detected in roflumilast.The established method is simple and sensitive with accurate and reliable detection results,which could be used for the detection of residual solvents in roflumilast raw material drug.
出处
《应用化工》
CAS
CSCD
2013年第8期1541-1543,共3页
Applied Chemical Industry
关键词
罗氟司特
残留溶剂
顶空气相色谱法
roflumilast
residual solvent
headspace gas chromatography
