顶空气相色谱法测定盐酸右美托咪定中3种有机溶剂残留量

Determination of three residual solvents in dexmedetomidine hydrochloride by headspace gas chromatography

目的建立顶空气相色谱法测定盐酸右美托咪定原料药中3种有机溶剂残留量的方法。方法用水溶解样品,采用顶空进样,在DB-WAX（25.0m×320μm×0.5μm）毛细管柱上程序升温,应用FID检测器,载气为氮气。结果甲醇、丙酮、二氯甲烷均能得到有效分离,各组分在考察的质量浓度范围内线性关系良好,r=0.999 0~0.999 9,平均回收率为96.2%~102.2%。结论该方法可用于检测盐酸右美托咪定原料药中甲醇、丙酮及二氯甲烷的残留量。

Objective To establish a headspace gas chromatography method for determining three kinds of residual solvents in dexmedetomidine hydrochloride.Methods The samples were dissolved by water,then the content of residual solvents was measured by headspace gas chromatography by using DB-Wax（25.0m×320μm×0.5μm）capillary column with sequential increasing of temperature.Nitrogen was used as the carrier gas with FID as a detector.Results The linearity（r=0.999 0-0.999 9）were satisfactory.Three residual solvents were completely separated,and the average recovery rates were between 96.2%-102.2%.Conclusion The method is simple,accurate and sensitive for the detection of three residual solvents in dexmedetomidine hydrochloride,and can be used for the quality control.