目的 采用超高效液相-三重四級桿質譜聯用技術(UPLC-MS/MS)對丁苯酞原料藥的雜質譜進行分析.方法 采用Waters ACQUITY UPLC^TM BEH C₁₈(50 mm×2.1 mm,1.7 μm)色譜柱,流動相為甲醇-0.1%甲酸溶液(60:40);Waters Quattro Premier XE QQQ質譜儀,離子源為ESI,檢測模式為正離子.結果 所有雜質均以丁苯酞的質譜裂解途徑為模板,進行了質譜解析,共確證了3個雜質的化學結構.結論 該研究對于丁苯酞原料藥的雜質分析、質量控制和合成工藝的改進具有重要作用.

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.

科技重大專項重大新藥創(chuàng)制(2015ZX09303001);科協新技術風險評估機制研究(2014ZCYJ03);農業(yè)部公益專項(201103027)