顶空毛细管GC法测定马波沙星原料药中6种溶剂的残留量

Determination of 6 Kinds of Residual Solvents in Marbofloxacin Bulk Drug by Headspace Capillary Gas Chromatography

建立顶空毛细管气相色谱法测定马波沙星原料药中甲醇、乙醇、乙腈、二氯甲烷、苯和甲苯等6种溶剂残留量。色谱柱为DB-624毛细管柱(30 m×0.53 mm,3.0μm),采用程序升温的方式,检测器为火焰离子化检测器(FID),检测器温度为250℃;顶空瓶平衡温度为105℃,平衡时间为20 min。结果显示,在该色谱条件下,6种溶剂均能得到良好分离;加样回收率均在100%~110%之间(RSD<8%,n=9),精密度重复性和稳定性结果均良好。该方法操作简便,重复性高,结果稳定可靠,可用于马波沙星残留溶剂的检测。

A method for the simultaneous determination of six kinds of residual solvents as methanol,ethanol,acetonitrile,dichromethane,benzene and toluene in marbofloxacin bulk drug was established by headspace gas chromatography.The residual solvents were seperated on DB-624(30 m×0.53 mm,3.0μm)capillary column using temperature programming.FID was used as detector with the temperature of 250℃.The sample was extracted at 105℃for 20 min.The results showed that the separation of six kinds of residual solvents was good.The average recoveries were ranged from 100%~110%(RSD<8%,n=9).Results of precision,repeatability and stability were good.Therefore,the established method which is simple,reproducible,stable and reliable can be used for detection of residual solvents in marboflocaxin bulk drug.