UPLC-QTOF-MS鉴定磺胺嘧啶原料药的有关物质

目的：对磺胺嘧啶原料药中12个有关物质进行结构鉴定。方法：采用高效液相色谱-四极杆飞行时间质谱技术推测各有关物质的结构。色谱条件：采用Waters BEH C₁₈色谱柱（2.1 mm×100 mm，1.7 μm），以乙腈-10 mmol·L^-1醋酸铵溶液（30：70）为流动相，流速0.2 mL·min^-1；质谱条件：采用正离子扫描（ESI⁺）方式，在m/z 50~1 000范围内进行质谱扫描；结合磺胺嘧啶与各有关物质的多级质谱裂解规律，鉴定各有关物质的结构。结果：获得了磺胺嘧啶原料药中12个有关物质的相对分子质量及结构式。结论：色谱-质谱联用技术能有效地鉴定磺胺嘧啶原料药中的有关物质，为其生产工艺和质量控制提供有意义的实验数据和参考依据。

Objetive: To elucidate the structure of 12 related substances in sulfadiazine by UPLC-QTOF-MS. Methods: UPLC-QTOF-MS was adopted to analyze the structure of the impurity based on the fragmentation behavior of sulfadiazine and its impurity. The separation was performed on a Waters BEH C₁₈ column (2.1 mm×100 mm,1.7 μm) with the mobile phase of a mixture of 30% acetonitrile and 70% 10 mmol·L^-1 ammonium acetate solution. Flow rate was 0.2 mL·min^-1. MS was performed under positive mode with the mass range of m/z 50-1 000. Results: The structures and molecular weights of the related substances in sulfadiazine were identified. Conclusion: The hyphenated LC-MS method is useful for the identification of related substances in sulfadiazine. The results obtained are valuable for its manufacturing process and quality control.

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