摘要
目的 建立一种快速鉴定益肺解毒颗粒的化学成分的高分辨质谱分析方法。方法 采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法(UHPLC-Q Exactive Focus MS/MS)对益肺解毒颗粒的成分进行快速鉴别,色谱柱为Thermo Accucore aQ C18色谱柱(2.1 mm×150 mm, 2.6μm),流动相为甲醇(A)-体积分数0.1%甲酸水溶液(B),梯度洗脱(0~3 min, 1%A;3~7 min, 1%~2%A;7~35 min, 2%~95%A;35~37 min, 95%~2%A;37~39 min, 1%A),柱温35℃,进样量3μL,流速0.3 mL·min-1。采用加热电喷雾离子源(HESI),在正、负离子同时扫描模式下采集益肺解毒颗粒的质谱数据,扫描范围m/z 100~1 500,碰撞能量30 eV。利用Xcalibur 4.1软件并结合对照品和文献信息,对益肺解毒颗粒的化学成分进行鉴定。结果 共鉴定出186个化学成分,包括三萜皂苷类38个、黄酮类34个、苯乙醇苷类17个、酚酸类14个、萜类16个、木脂素类11个、色原酮类11个、香豆素类10个、酚酸甘油酯类9个、挥发油类3个、核苷类3个、糖类2个、酚类2个、氨基酸类1个、其他类15个。其中10个化合物通过对照品比对进行了确证。结论 该方法可对益肺解毒颗粒中化学成分进行快速、准确地鉴定和分析,为其质量评价、药效物质及作用机制等研究奠定了基础。
OBJECTIVE To establish a high-resolution mass spectrometry method for rapid identification of chemical constituents of Yifei Jiedu Granules.METHODS The composition of Yifei Jiedu Granules was rapidly identified by ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitwell high resolution mass spectrometry(UHPLC-Q Exactive Focus MS/MS).The analysis was performed on Thermo Accucore aQ C18 column(2.1 mm×150 mm,2.6μm)with mobile phase of methanol(A)-0.1%formic acid(B)for gradient elution(0-3 min,1%A;3-7 min,1%-2%A;7-35 min,2%-95%A;35-37 min,95%-2%A;37-39 min,1%A).The column temperature was at maintained 35℃,the injection volume was 3μL and the flow rate was 0.3 mL·min-1.The information of the chemical constituents of Yifei Jiedu Granules was acquired in positive and negative ion modes by heated electrospray ion source(HESI),scanning range of 100-1500 m/z,and collision energy of 30 eV.The chemical constituents of Yifei Jiedu Granules were identified by Xcalibur 4.1 software combined with reference and literature information.RESULTS A total of 186 chemical components were identified,including 38 triterpenoid saponins,34 flavonoids,17 phenylethanolsides,14 phenolic acids,16 terpenoids,11 lignans,11 chromogenic ketones,10 coumarins,9 phenolic triglycerides,3 volatile oils,3 nucleosides,2 sugars,2 phenols,1 amino acid and 15 other groups.Ten of the compounds were confirmed by comparison with reference materials.CONCLUSION The established method can be used for rapid and accurate identification and analysis of chemical constituents in Yifei Jiedu Granules,which lays a foundation for quality evaluation and research on pharmacodynamic substances and mechanism of action.
作者
刘静
龙凯花
马战平
杜霞
张红
LIU Jing;LONG Kaihua;MA Zhanping;DU Xia;ZHANG Hong(Shaanxi Academy of Traditional Chinese Medicine,Xi'an 710003,China;Shaanxi Hospital of Chinese Medicine,Xi'an 710003,China)
出处
《中国药学杂志》
CAS
CSCD
北大核心
2023年第21期1940-1954,共15页
Chinese Pharmaceutical Journal
基金
陕西省重点研发计划项目资助(2022ZDXM-SF-06,2022SF-273)
陕西省中医药管理局项目资助(2021-ZZ-JC022)
西安市科技计划项目资助(21YXYJ97)。
作者简介
刘静,女,研究实习员研究方向:中药药效物质基础研究;通讯作者:杜霞,女,博士,副研究员研究方向:中药药效物质基础研究,Tel:(029)85413239;通讯作者:张红,女,博士,研究员研究方向:中药药效物质基础研究,Tel:(029)85395696。
