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UPLC-Q-TOF-MS/MS法快速定性分析通脉养心丸中的化学成分
魏娟1, 姚广哲1, 欧阳慧子2, 常艳旭1, 何俊1
1.天津中医药大学, 天津市现代中药重点实验室, 天津 301617;2.天津中医药大学第一附属医院, 天津 300193
摘要:
[目的]采用超高效液相色谱串联飞行时间质谱法定性分析通脉养心丸中的化学成分。[方法]分析采用ACQUITY UPLC® BEH C18色谱柱(2.1 mm×100 mm,1.7 μm),流动相为0.1%甲酸水溶液-乙腈,梯度洗脱,流速为0.3 mL/min,柱温30℃;分别在正、负离子模式下进行数据采集,通过与标准品对比保留时间、相对分子质量,结合二级碎片裂解规律,以及相关文献核对的方法确定化学成分。[结果]在正负离子模式下共鉴定出了32个化合物,包括黄酮类、皂苷类、蒽醌类、木质素类、有机酸类等化合物。[结论]本方法可以快速全面的定性分析通脉养心丸中的化学成分,为通脉养心丸的质量控制和药效物质基础的阐明提供参考。
关键词:  通脉养心丸  UPLC-Q-TOF-MS/MS  定性分析  化学成分
DOI:10.11656/j.issn.1673-9043.2019.04.19
分类号:R284.2
基金项目:国家自然科学基金项目资助(81673824)。
Rapid qualitative analysis of chemical constituents in Tongmai Yangxin pill by UPLC-Q-TOF-MS/MS
WEI Juan1, YAO Guangzhe1, OUYANG Huizi2, CHANG Yanxu1, HE Jun1
1.Tianjin University of Traditional Chinese Medicine, Tianjin University of Traditional Chinese Medicine, Tianjin 301617, China;2.First Teaching Hospital of Tianjin University of Traditional Chinese Medicine, Tianjin 300193, China
Abstract:
[Objective] To use a qualitative analytical method of ultra-high performance liquid coupled with quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS/MS) for identification chemical constituents in Tongmai Yangxin pill.[Methods] The assay was performed on an ACQUITY UPLC® BEH C18 column (2.1 mm×100 mm, 1.7 μm) with the mobile phase consisting of water containing 0.1% formic acid (A) and acetonitrile (B) in gradient mode at a flow rate of 0.3 mL/min, The column temperature was at 30℃;Data acquisition was carried out under positive and negative ion modes, and chemical composition was determined by comparing retention time and relative molecular mass with standard products, combining with secondary fragment fragmentation law and related literature.[Results] Thirty-two compounds including flavonoids, saponins, terpenoids and anthraquinones were identified under positive and negative ion modes.[Conclusion] This method can be used for rapid and comprehensive qualitative analysis of chemical constituents in Tongmai Yangxin pills, providing reference for quality control of Tongmai Yangxin pills and elucidation of pharmacodynamic material basis.
Key words:  Tongmai Yangxin pill  UPLC-Q-TOF-MS  qualitative analysis  chemical constituents
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