Chinese Journal of Chromatography ›› 2015, Vol. 33 ›› Issue (1): 22-28.DOI: 10.3724/SP.J.1123.2014.07006

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An ultra-high-pressure liquid chromatography/linear ion trap-Orbitrap mass spectrometry method coupled with a diagnostic fragment ions-searching-based strategy for rapid identification and characterization of chemical components in Polygonum cuspidatum

PAN Zhiran1, LIANG Hailong1, LIANG Chaohui1, XU Wen1,2   

  1. 1. The Second College of Clinic Medicine, Guangzhou University of Chinese Medicine, Guangzhou 510006, China;
    2. Guangdong Province Institute of Chinese Medicine, Guangzhou 510006, China
  • Received:2014-07-02 Revised:2014-09-16 Online:2015-01-08 Published:2014-12-26

Abstract:

A method for qualitative analysis of constituents in Polygonum cuspidatum by ultra-high-pressure liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometry (UHPLC-LTQ-Orbitrap MS) has been established. The methanol extract of Polygonum cuspidatum was separated on a Waters UPLC C18 column using acetonitrile-water (containing formic acid) eluting system and detected by LTQ-Orbitrap hybrid mass spectrometer in negative mode. The targeted components were further fragmented in LTQ and high accuracy data were acquired by Orbitrap MS. The summarized fragmentation pathways of typical reference components and a diagnostic fragment ions-searching-based strategy were used for detection and identification of the main phenolic components in Polygonum cuspidatum. Other clues such as nitrogen rule, even electron rule, degree of unsaturation rule and isotopic peak data were included for the structural elucidation as well. The whole analytical procedure was within 10 min and more than 30 components were identified or tentatively identified. This method is helpful for further phytochemical research and quality control on Polygonum cuspidatum and related preparations.

Key words: Polygonum cuspidatum, chemical components, LTQ-Orbitrap mass spectrometry, traditional Chinese medicine, ultra-high-pressure liquid chromatography (UHPLC)

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