UPLC-MS/MS法研究丁苯酞原料药的杂质谱

Study on impurity profiling of butylphthalide by UPLC-MS/MS

目的采用超高效液相-三重四级杆质谱联用技术(UPLC-MS/MS)对丁苯酞原料药的杂质谱进行分析。方法采用Waters ACQUITY UPLCTM BEH C18(50 mm×2.1 mm,1.7μm)色谱柱,流动相为甲醇-0.1%甲酸溶液(60∶40);Waters Quattro Premier XE QQQ质谱仪,离子源为ESI,检测模式为正离子。结果所有杂质均以丁苯酞的质谱裂解途径为模板,进行了质谱解析,共确证了3个杂质的化学结构。结论该研究对于丁苯酞原料药的杂质分析、质量控制和合成工艺的改进具有重要作用。

Objective Investigation of butylphthalide and its related substances was carried out using a reversed phase ultra performance liquid chromatography/tandem mass spectrometry method. Methods Separation was performed on Waters ACQUITY UPLCTM BEH C18(2.1 mm × 50 mm, 1.7 μm), the mobile phase consisted of methanol-0.1% formic acid in water(60:40); The identification of impurities in butylphthalide was performed with a triple-quadrupole mass spectrometer, with an electrospray ionization(ESI) source in the positive ion mode. Results All the impurities were deduced based on the MS fragment pathways of butylphthalide, a total of three compounds were characterized. Conclusion This work provides useful information for studying the origin of the impurities of butylphthalide and quality control of butylphthalide.