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 UPLC^TM BEH C₁₈(50 mm×2.1 mm,1.7 μm)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 UPLC^TM 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.

科技重大专项重大新药创制(2015ZX09303001);科协新技术风险评估机制研究(2014ZCYJ03);农业部公益专项(201103027)