HPLC-MS/MS测定达卡巴嗪有关物质___

目的: 采用液质联用分析技术,对达卡巴嗪有关物质进行分析。 方法: 采用高效液相色谱-电喷雾离子化-质谱联用法,色谱柱为Shim-pack CLC-ODS(250 mm×4.6 mm,5 μm)柱,以冰醋酸-水(6∶ 94,用氨试液调节pH至3.0)为流动相,流速1.0 mL·min^-1,柱后分流,进样量10 μL,DAD检测器,检测波长254 nm。电喷雾电离源(ESI),电离源电压4.0 kV,喷雾气氮气的流速为9.0 L·min^-1,干燥气温度为325 ℃;质谱扫描质量范围m/z 50~1200。采用全扫描一级质谱和选择离子全扫描二级质谱(MS/MS)2种方式同时测定。 结果 :分析了达卡巴嗪的2个主要降解产物的结构。 结论: 已有国家药品标准收载的达卡巴嗪及其制剂质量标准中有关物质检查项下应增加对降解产物的控制。

Objective: To establish an HPLC-MS/MS determination method to analyze the related substance of dacarbazine. Methods: The HPLC-ESI-MS/MS on Shim-pack CLC-ODS column(250 mm×4.6 mm,5 μm) was adopted;The mobile phase consisted of glacial acetic acid-water(6∶ 94,adjust the solution to pH 3.0 with ammonia water) at the flow rate of 1.0 mL·min^-1;The diode-array detector wavelength was set at 254 nm.Ion trap mass spectrum,spray capillary voltage was 4.0 kV,flow rate of dry gas N₂ was 9.0 L·min^-1,dry gas temperature was set at 325 ℃,and scan range was m/z 50-1200;Samples were analyzed in two modes:MS and MS/MS full scan modes. Results: The structures of two main decomposition compounds of dacarbazine were analyzed. Conclusion: It’s essential to control the degradation compounds of dacarbazine.