目的: 以超高效液相色谱-四极杆-高分辨轨道阱液质联用技术为主要手段,结构定性黄藤素中的3个降解杂质。方法: 采用Thermo Gold C18色谱柱(100 mm×2.1 mm, 1.9 μm),以水-乙腈-甲酸(82∶18∶0.1)为流动相,流速为0.3 mL·min-1,柱温为30 ℃;离子源为HESI离子源,扫描模式为正离子扫描,碎片分析借助MsFrontier 7.0软件。结果: 通过HPLC-DAD、UPLC-HRMS等手段,结合有机反应理论鉴定黄藤素杂质谱中的3个降解杂质,分别为5-羟基黄藤素(杂质2)、10-羟基黄藤素(杂质4)和2-羟基黄藤素(杂质5)。结论: 该研究为黄藤素的质量控制和安全性评价奠定基础。
Objective: To confirm the structures of three degradation impurities in fibriuretinin using UPLC-Q-Orbitrap HRMS. Methods: UPLC was applied with a Thermo Gold C18 column (100 mm×2.1 mm, 1.9 μm) and eluted with water-acetonitrile-formic acid (82∶18∶0.1) as mobile phase under the condition of flow rate 0.3 mL·min-1 and column temperature 30 ℃. MS was applied with HESI source and positive ion modes. Fragment analysis was carried out with MsFrontier 7.0 software. Results: Three degradation impurities, which were 5-hydroxy-fibriuretinin (impurity 2), 10-hydroxy-fibriuretinin (impurity 4), and 2-hydroxy-fibriuretinin (impurity 5), were confirmed by methods such as HPLC-DAD, UPLC-HRMS combined with organic reaction theory. Conclusion: The study of the structures of the degradation impurities provides a reference for the quality control and safety evaluation of fibriuretinin.
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