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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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UPLC-QTOF-MS鉴定磺胺嘧啶原料药的有关物质

Identification of related substances in sulfadiazine by UPLC-QTOF-MS

作者: 李璐, 廖乃英 
作者(英文):
分类号:R917
出版年·卷·期(页码):2019,39 (12):2148-2156
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

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。

-----英文摘要:---------------------------------------------------------------------------------------

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.

-----参考文献:---------------------------------------------------------------------------------------

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