[关键词]
[摘要]
目的:采用高效液相色谱串联四极杆-静电场轨道阱高分辨质谱(HPLC-Q-Exactive-MS/MS)对朱日亨滴丸及其中间体中的化学成分进行快速鉴定和归属。方法:选用ACE EXCEL3 C18-PFP 色谱柱(3μm,100mm×3mm),流动相为含0.2%甲酸的甲醇(A)-0.2%甲酸水溶液(B),梯度洗脱,流速0.3mL.min-1,柱温35℃。正、负离子模式采集数据,质谱扫描范围为m/z 100~1000。通过文献检索、中药材网站收集朱日亨滴丸原药材中化学成分,自建化学成分数据库。根据精确相对分子质量、二级质谱裂解碎片、对照品及文献比对,对朱日亨滴丸及中间体中化学成分进行鉴定。结果:共识别和鉴定了朱日亨滴丸中130个成分,包括18个苯丙素、24个木脂素、26个黄酮、10个香豆素、13个环烯醚萜、15个有机酸、14个酚酸、8个单萜、2个其他类成分。结论:建立的HPLC-Q-Exactive-MS/MS方法快速、准确。适用于朱日亨滴丸及其中间体的定性鉴别。为该药的质量体系建立和药效物质发现奠定了基础。
[Key word]
[Abstract]
Object: Rapid high performance liquid chromatography tandem quadrupole-electrostatic field orbitrap high resolution mass spectrometry(HPLC-Q-Exactive-MS/MS)was used to rapidly analyze and assign the chemical constituents of Zhuriheng pills and their intermediate products. Method: ACE EXCEL3 C18-PFP (3μm, 100mm×3mm) column was selected for chromatographic analysis, the mobile phase was methanolcontaining 0.2% formic acid (A) -0.2% formic acid aqueous solution (C) for gradient elution, flow rate was 0.3mL.min-1, and the column temperature was 35°C. Mass spectrometry data were collected in positive and negative ion modes, and the scanning range of the mass spectrum was m/z 100~1000. The chemical constituents of Zhuriheng pills were speculated and identified according to the precise molecular weight, secondary fragmentation, literature data and compared with standard substance. Result: A total of 130 compounds in Zhuriheng pills were identified and speculated in positive and negative ion mode, including 18 phenylpropanoids, 24 lignans, and 26 Flavonoids, 10 coumarins, 13 iridoids, 15 organic acids, 14 phenolic acids, 8 monoterpenes, and 2 other compounds. Conclusion: The established method is rapid and accurate. It is suitable for the qualitative identification of Zhuriheng dripping pills and their intermediates. It laid the foundation for the quality evaluation system and the discovery of effective substances.
[中图分类号]
[基金项目]
国家自然科学基金(81960757);内蒙古科技成果转化项目(2019CG042);内蒙古自然科学基金(2019MS08119)