中国药物警戒 ›› 2021, Vol. 18 ›› Issue (9): 831-836.
DOI: 10.19803/j.1672-8629.2021.09.08

• 基础与临床研究 • 上一篇    下一篇

基于UPLC-ESI-QTOF-MS/MS技术检测扶正固本颗粒化学成分

仝立国1, 牛艳艳1, 贾力莉1, 王若瑜1, 宋美卿1, 夏召弟1, 冯玛莉1, 汪欣文1,*, 吉海杰1,2#   

  1. 1山西省中医药研究院,山西 太原 030012;
    2中国中医科学院博士后流动站,北京 100700
  • 收稿日期:2020-03-19 出版日期:2021-09-15 发布日期:2021-09-18
  • 通讯作者: *汪欣文,硕士,副主任医师,肿瘤内科学。E-mail：zf-xfdy@163.com,# 为共同通信作者。
  • 作者简介:仝立国,硕士,副主任药师,中药药效物质基础及质量标准研究。
  • 基金资助:
    国家自然科学基金资助项目（81973672）; 山西省科技攻关项目山西省中药现代化关键技术研究振东专项（2016ZD0302）; 中国博士后科学基金面上项目（2016M590186）; 山西省中医药管理局科研课题（2019ZYYC005,2020ZYYZ010）; 山西中医药大学科技创新能力培育计划项目（2019PY-020）

Identification of Chemical Substances in Fuzheng Guben Granules Based on UPLC-ESI-QTOF-MS/MS Technique

TONG Liguo1, NIU Yanyan1, JIA Lili1, WANG Ruoyu1, SONG Meiqing1, XIA Zhaodi1, FENG Mali1, WANG Xinwen1,*, JI Haijie1,2#   

  1. 1Shanxi Academy of Traditional Chinese Medicine, Taiyuan Shanxi 030012, China;
    2Postdoctoral Research Station, China Academy of Chinese Medical Sciences, Beijing 100700, China
  • Received:2020-03-19 Online:2021-09-15 Published:2021-09-18

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摘要： 目的 基于超高效液相色谱-电喷雾离子源-四极杆飞行时间质谱联用技术（UPLC-ESI-QTOF-MS/MS）检测扶正固本颗粒中的化学成分并进行确认。方法 采用ACQUITY UPLC HSS T3 C18色谱柱（2.1 mm×100 mm,1.8 μm),以0.1%甲酸甲醇溶液（A）-0.1%甲酸水溶液（B）为流动相梯度洗脱,流速0.2 mL/min,柱温40 ℃,同时联合XEVO G2-XS ESI离子源进行正、负离子模式测定,通过比对保留时间、分子精确质量数及二级质谱碎片等参数,结合UNIFI软件分析各成分碎片裂解方式并参考化学成分数据库及文献数据对检测到的化学成分进行确认鉴定。结果 初步鉴定出56个化合物,其中包括黄酮类化合物29个,蒽醌类化合物9个,二苯乙烯苷类化合物2个,萜类化合物6个,皂苷类化合物3个及7个其他成分。结论 该方法可快速、准确的鉴定出扶正固本颗粒中的多种化学成分,为寻找其药效物质基础及进一步建立全面质量控制方法提供了依据。

关键词: 扶正固本颗粒, 超高效液相色谱仪, 电喷雾离子源, 四极杆飞行时间质谱

Abstract: Objective To analyze the chemical constituents in Fuzheng Guben granules using ultra performance liquid chromatography electrospray ion source quadrupole time of flight mass spectrometry (UPLC-ESI-QTOF-MS/MS). Methods The chromatographic column of Acquity UPLC HSS T3 C18 (2.1×100 mm, 1.8 μm) was used. The mobile phase was 0.1% formic acid methanol solution (A)-0.1% formic acid aqueous solution (B) in gradient elution, the flow rate 0.2 ml/min, and the column temperature was 40 ℃. The positive and negative ion modes of each component were determined respectively by Xevo G2-XS ESI ion source. According to such parameters as the retention time, molecular accurate mass number and secondary mass spectrum fragments, Unifi software was used to analyze the fragmentation mode of each component, while the reference chemical component database and literature data were used to analyze the detected chemical components. Results Fifty-six compounds were identified, including 29 flavonoids, 9 anthraquinones, 2 stilbene glycosides, 6 terpenes, 3 saponins and 7 other components. Conclusion This method can identify various chemical components of Fuzheng Guben granules quickly and accurately, which provides data for finding effective substances and establishing methods for total quality control.

Key words: Fuzheng Guben granules, UPLC, ESI, QTOF

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