色谱

色谱 ›› 2020, Vol. 38 ›› Issue (5): 554-563.DOI: 10.3724/SP.J.1123.2019.10006

• 研究论文 • 上一篇    下一篇

利用在线加压溶剂提取-超高效液相色谱-离子肼-飞行时间-质谱法直接分析中药草苁蓉的化学成分组

李婷1, 许霞1, 常安琪1, 刘文静1, 宋青青1,*(), 宋月林1,2,*(), 屠鹏飞1   

  1. 1 北京中医药大学中药学院中药现代研究中心, 北京 100029
    2 中药品质评价北京市重点实验室, 北京 100029
  • 收稿日期:2019-10-10 出版日期:2020-05-08 发布日期:2020-12-10
  • 通讯作者: 宋青青,宋月林
  • 作者简介:宋月林.Tel:01064286100, E-mail:syltwc2005@163.com
    宋青青.Tel:01064286100, E-mail:sqq1991qq@163.com;
  • 基金资助:
    国家自然科学基金项目(81773875);国家自然科学基金项目(81530097);中国科协青-人才托举工程(2017QNRC001);国家重点研发计划(2018YFC1707300);国家重点研发计划(2017YFC702400)

Direct chemome profiling of Boschniakia rossica using online pressurized extraction-ultrahigh-performance liquid chromatography-ion trap-time-of-flight mass spectrometry

LI Ting1, XU Xia1, CHANG Anqi1, LIU Wenjing1, SONG Qingqing1,*(), SONG Yuelin1,2,*(), TU Pengfei1   

  1. 1 Modern Research Center for Traditional Chinese Medicine, School of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing 100029, China
    2 Beijing Key Lab for Quality Evaluation of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing 100029, China
  • Received:2019-10-10 Online:2020-05-08 Published:2020-12-10
  • Contact: SONG Qingqing,SONG Yuelin
  • Supported by:
    National Natural Science Foundation of China(81773875);National Natural Science Foundation of China(81530097);Young Talents Lifting Project from China Association for Science and Technology(2017QNRC001);National Key Research & Development Program of China(2018YFC1707300);National Key Research & Development Program of China(2017YFC702400)

RichHTML

7

PDF

42

摘要：

构建了在线加压溶剂提取-超高效液相色谱-离子肼-飞行时间质谱（online PLE-UHPLC-IT-TOF-MS）系统，并将其应用于草苁蓉化学组的快速、直接分析。将微量草苁蓉粉末（0.5 mg）置于空预柱芯中，空隙用正相硅胶填充，作为提取池；提取池置于预柱套内，将其放入柱温箱（70℃），预柱套通过金属管线连接至UHPLC-IT-TOF-MS系统。通过引入一个二位六通阀将整个分析过程分为提取和洗脱两个阶段。以0.1%（v/v）甲酸水为溶剂，提取3 min。在洗脱阶段，以0.1%（v/v）甲酸水-0.1%（v/v）甲酸乙腈为流动相，梯度洗脱，将色谱柱前端所富集的提取物洗脱至IT-TOF-MS中进行检测。从草苁蓉中检测到48个化合物，结合对照品、文献、数据库以及质谱裂解规律，初步鉴定了其中的45个，包括10个苯乙醇苷类、14个环烯醚萜苷类以及21个苯丙醇苷类化合物。该研究为草苁蓉化学成分组成的阐明以及质量评价提供了可靠信息。同时，构建的online PLE-UHPLC-IT-TOF-MS系统为中药化学成分的快速、直接表征提供了有效方案。

关键词: 在线加压溶剂提取, 草苁蓉, 化学成分组, 质谱裂解规律, 苯丙醇苷

Abstract:

An online pressurized extraction-ultrahigh-performance liquid chromatography-ion trap-time-of-flight mass spectrometry (online PLE-UHPLC-IT-TOF-MS) platform was configured for the rapid and direct profiling of the chemical constituents of Boschniakia rossica (B. rossica). Notably, only a sub-microgram amount (0.5 mg) of B. rossica was placed in an empty guard column core, which was then filled up with normal-phase silica gel as an extraction vessel. The guard column core was placed inside a guard column holder in the column oven (70℃) and connected to the UHPLC-IT-TOF-MS system via metal tubing. The extraction phase was maintained for 3 min with 0.1% (v/v) formic acid as the extraction solvent. The extraction and elution phases for the entire measurement were segmented by a 6-port/2-channel electronic valve. In the elution phase, 0.1% (v/v) aqueous formic acid-acetonitrile containing 0.1% (v/v) formic acid was the mobile phase, and the components of interest that accumulated at the front of the column were eluted into the IT-TOF-MS system for detection. A total of 48 compounds were observed, and according to the literature, database, and mass fragmentation pathways, 45 compounds, including 10 phenylethanol glycosides, 14 iridoid glycosides, and 21 phenylalanine glycosides, were identified from B. rossica. This study provides reliable information regarding the chemical composition and quality evaluation of B. rossica. Moreover, it offers a promising analytical pipeline for the chemical composition characterization of traditional Chinese medicines.

Key words: online pressurized liquid extraction, Boschniakia rossica (B. rossica), chemome profiling, mass fragmentation pathways, phenylpropanoid glycosides