顶空气相色谱法测定托拉塞米中7种有机溶剂残留量

Determination of seven residual organic solvents in torasemide by headspace capillary gas chromatography

目的建立托拉塞米中9种有机溶剂残留量的测定方法。方法采用顶空毛细管气相色谱法,以二甲基亚砜为溶剂,DB-624色谱柱(30m×0.32mm×0.250μm),FID检测器。结果 7种残留有机溶剂甲醇、乙醇、丙酮、二氯甲烷、正丙醇、二氧六环、甲苯均达到了完全分离。结论该方法灵敏度、准确度均达到有机溶剂残留量的检测要求,可用于托拉塞米中7种残留溶剂的同时检测。

OBJECTIVE To develop a headspace capillary gas chromatography for determining the residual organic solvents methanol,ethanol,acetone,dichloromethane,n-propanol,dioxane and toluene in torasemide.METHODS The samples were dissolved in dimethyl sulfoxide.The nine organic solvents were separated on a DB-624 capillary colunn（30m×0.32mm×0.250μm）using programmable increased temperature.The intial temperature was kept at 40℃ for 30min.The temperature was raised to 180℃ at the rate of 20℃·min-1.RESULTS Seven residual organic solvents consisting of methanol,ethanol,acetone,dichloromethane,n-propanol,dioxane and toluene in Torasemide were completely separated,and the samples coincided with the requirements.CONCLUSION The methods was proved to be accurate and sensitive after validation.It is suitable to the determination of residual organic solvents in Torasemide.