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LC-Q-TOF/MS技术鉴定阿替洛尔中氨基醇类有关物质

齐文竹, 邹桐, 管艺同, 宋敏, 杭太俊

齐文竹, 邹桐, 管艺同, 宋敏, 杭太俊. LC-Q-TOF/MS技术鉴定阿替洛尔中氨基醇类有关物质[J]. 中国药科大学学报, 2020, 51(5): 544-555. DOI: 10.11665/j.issn.1000-5048.20200506
引用本文: 齐文竹, 邹桐, 管艺同, 宋敏, 杭太俊. LC-Q-TOF/MS技术鉴定阿替洛尔中氨基醇类有关物质[J]. 中国药科大学学报, 2020, 51(5): 544-555. DOI: 10.11665/j.issn.1000-5048.20200506
QI Wenzhu, ZOU Tong, GUAN Yitong, SONG Min, HANG Taijun. Identification of amino alcohols related substances of atenolol by LC-Q-TOF/MS[J]. Journal of China Pharmaceutical University, 2020, 51(5): 544-555. DOI: 10.11665/j.issn.1000-5048.20200506
Citation: QI Wenzhu, ZOU Tong, GUAN Yitong, SONG Min, HANG Taijun. Identification of amino alcohols related substances of atenolol by LC-Q-TOF/MS[J]. Journal of China Pharmaceutical University, 2020, 51(5): 544-555. DOI: 10.11665/j.issn.1000-5048.20200506

LC-Q-TOF/MS技术鉴定阿替洛尔中氨基醇类有关物质

Identification of amino alcohols related substances of atenolol by LC-Q-TOF/MS

  • 摘要: 研究鉴定阿替洛尔中氨基醇类有关物质。阿替洛尔及其强制降解样品中的有关物质采用9-芴甲氧羰酰氯柱前衍生化,以Inertsil ODS-SP (250 mm×4.6 mm,5 μm)色谱柱,甲醇-乙酸铵缓冲液为流动相进行梯度洗脱分离,电喷雾正离子化-高分辨Q-TOF/MS测定这些有关物质衍生物的母离子及碎片离子的准确质量和元素组成,经光谱解析和合成路线分析鉴定各有关物质结构。所建立的方法,阿替洛尔及其氨基醇类有关物质均分离良好,共检测并鉴定出14个杂质峰,其中12个为有关物质,2个为衍生化反应副产物。建立的LC-MS方法可为阿替洛尔有关物质检查和质量控制提供参考依据。
    Abstract: To identify the amino alcohols related substances in atenolol. The related substances in atenolol and its stressed samples were pre-column derivatized with 9-fluorenylmethyl chloroformate. The separation was carried out on an Inertsil ODS-SP column (250 mm×4.6 mm, 5 μm) with linear gradient elution by methanol-ammonium acetate solution as the mobile phases. Electrospray positive ionization high-resolution Q-TOF/MS was used for the determination of the accurate masses and elemental compositions of the parent and fragment ions of these related substance derivatives. The structures of all the detected substances were identified by spectral analysis and synthetic analysis. Under the established conditions, atenolol and its amino alcohols related substances were well separated, and a total of 14 impurity peaks were detected and identified, of which 12 were related substances and 2 were derivatization reaction by-products. The established LC-MS method provides a reference for the examination and quality control of atenolol related substances.
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出版历程
  • 收稿日期:  2020-04-10
  • 修回日期:  2020-06-08
  • 刊出日期:  2020-10-24

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